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0 RN L-4343 UC-4 - Chemistry

Contract No. W-7405-eng-26

ANALYTICAL CHEMISTRY DIVI SI ON ANNUAL PROGRESS REPORT

For Period Ending September 30, 1968

M. T. Kelley, Director J. C. White, Associate Director

Compiled and Edited by Helen P. Raaen

DECEMBER 1968

OAK RIDGE NATIONAL LABORATORY Oak Ridge, Tennessee operated by UNION CARBIDE CORPORATION for the U. S. ATOMIC ENERGY COMMISSION

LEGAL NOTICE This report nas prepared as an account of Government sponsored work. Neither the United States. nor the Commission. nor any person acting on behalf of the Commlsslon: A. Makes any warranty or representation. expressed or implied. with respect to the accu- racy, completeness, or usefulness of the idarmation contained in this report. or that the use of any information, apparatus, method, or process disclosed In this report may not infringe privately owned rights: or B. Aasumes any liabilities with respect to the use of, or for damages resulting from the use of any information, apparatus, method, or process disclosed in this report. As used in the above. "person acting on behalf of the Commission" Includes any em- ployee or contractor of the Commission. or employee of such contractor. to the extent that such employee or contractor of the Commlsslon. or employee of such contractor prepares. disseminates. or provides access to, any information pursuant to his employment or contract wlth the Commission, or his employment with such contractor. DISCLAIMER

This report was prepared as an account of work sponsored by an agency of the United States Government. Neither the United States Government nor any agency Thereof, nor any of their employees, makes any warranty, express or implied, or assumes any legal liability or responsibility for the accuracy, completeness, or usefulness of any information, apparatus, product, or process disclosed, or represents that its use would not infringe privately owned rights. Reference herein to any specific commercial product, process, or service by trade name, trademark, manufacturer, or otherwise does not necessarily constitute or imply its endorsement, recommendation, or favoring by the United States Government or any agency thereof. The views and opinions of authors expressed herein do not necessarily state or reflect those of the United States Government or any agency thereof. DISCLAIMER

Portions of this document may be illegible in electronic image products. Images are produced from the best available original document.

Reports previously issued in this series are as follows:

ORNL-686 Period Ending March 3 1, 1950 OWL-788 Period Ending June 30, 1950 ORNL-867 Period Ending October 10, 1950 ORNL-955 Period Ending January 10,1951 ORNL-1088 Period Ending March 26, 1951 OWL-1113 Period Ending June 26, 195 1 ORNL-1129 Period Ending September 10, 1951 ORNL-1233 Period Ending December 26, 1951 ORNL-1276 Period Ending March 26, 1952 ORNL- 136 1 Period Ending June 26, 1952 ORNL- 1423 Period Ending September 26, 1952 ORNL-1474 Period Ending January 10,1953 ORNL-1547 Period Ending April 20, 1953 ORNL-1639 Period Ending October 20, 1953 ORNL-1717 Period Ending April 20, 1954 OWL-1788 Period Ending October 20, 1954 ORNL-1880 Period Ending April 20, 1955 0RNL- 19 73 Period Ending October 20, 1955 ORNL-2070 Period Ending April 20, 1956 ORNL-2218 Period Ending December 3 1, 1956 ORNL-2453 Period Ending December 3 1, 1957 ORNL-2662 Period Ending December 3 1, 1958 ORNL-2866 Period Ending December 3 1, 1959 ORNL-3060 Period Ending December 3 1, 1960 ORNL-3243 Period Ending December 3 1, 196 1 ORNL-3397 Period Ending December 3 1, 1962 ORNL-3537 Period Ending November 15, 1963 ORNL-375 0 Period Ending November 15, 1964 ORNL-388 9 Period Ending November 15, 1965 ORNL-4039 Period Ending October 3 1, 1966 ORNL-4196 Period Ending October 3 1, 1967 Preface

The general mission of the Analytical Chemistry Division is to provide complete analytical support for the many research programs at ORNL. This support comprises research in analytical chemistry, development of new and improved methods for analysis, and a chemical analysis service that employs a wide variety of analytical techniques. The great diversity in the research programs at ORNL is likewise reflected in a similar diversity in the activities of the Division. The research and development efforts within the Division are oriented toward providing the most suitable analytical techniques for the analyses that the Division is called upon to perform. Efforts are made constantly to provide more precise and more rapid analyses by employing the most advanced instrumentation available and by using automated or semiautomated procedures. Efforts are being made to use electronic data acquisition and processing equipment wherever possible. Considerable progress has been made in this regard this year in that three small dedicated computers have been acquired and commitments have been made for the acquisition of two more such devices. Initially, these will be used primarily for acquisition of data in digital form, but at least one of these will be used to explore the feasibility of computer-controlled analytical instrumentation. It is gratifying to note that the preeminence of the work of the Division in the field of analytical instrumentation has been recognized by the announcement that Dale J. Fisher, Croup Leader of the Analytical Instrumentation Group, will be the recipient of the 1969 ACS Award in Chemical Instrumentation sponsored by the Sargent-Welch Scientific Company. The Division is continuing major research and development programs with the objectives of providing chemical analyses for the MSRE and for bioengineering programs. Efforts in analytical biochemistry continue to occupy a major place in the program of the Division with constant exploration being made of areas that would constitute a logical expansion of present work in this field. This emphasis is in recognition of the increasing importance of biology and biochemistry in the research efforts of ORNL and of the entire scientific community.

... 111 8' . Contents

... PREFACE ...... 111

SUMMARY ...... xiii

PART A . ANALYTICAL RESEARCH

1. ANALYTICAL INSTRUMENTATION ...... 1 J 1.1 Solid-state Controlled-Potential Coulometric Titrator ...... 1 1.2 Modifications to the High-Sensitivity Controlled-Potential Coulometric Titrator (ORNL Model Q-2564) ...... 2 1.3 Instrumentation for the High-Radiation-Level Analytical Laboratory (HRLAL) ...... 2 1.3.a New Titrant-Delivery Unit and Elevator ...... 2 1.3.b New ORNL Model Q-1348C Pipetter ...... 2 1.4 Apparatus for Precise Control of Flow Rate of Dropping-Mercury Electrodes (D.M.E.’s) ...... 2 1.5 Electrical and Electrochemical Tests of Performance of Polarographs ...... 2

1.6 A Controlled-Potential and Derivative DC Polarograph - Advantages of Kapid and Derivative DC Polarography ...... 3 1.7 Polarography of in Acetonitrile and Dimethyl Sulfoxide ...... 3 1.8 Polarographic Survey of Biochemicals ...... 4 1.9 ORNL Model Q-2792 Controlled-Potential DC Polarograph and ORNL Model Q-2942 Polarographic Drop-Time Controller ...... 5 1.10 Design of Time-Averaging and Time-Derivative Circuits for DC Polarographs ...... 5 1.1 1 Instrument for End-Point Detection in Bipotentiometric Titrations ...... 5 1.1 2 Controlled-Potential Controlled-Current Cyclic Voltammeter ...... 6 1.1 3 Derivative Circuits for Use with the Controlled-Potential Controlled-Current Cyclic Voltammeter ...... 6 1. 14 On the Separation of Half-Wave Potentials Required for Resolution of Simple, Reversible, Overlapping Waves in Stationary-Electrode Voltammetry ...... 7 1.1 5 Modification of Dual Set-Point Voltage Comparator (ORNL Model Q-2950) ...... 7 1.16 Integrator Module ...... 7 - 1.17 Model IX Flame Spectrophotometer ...... 7 1.1 8 Use of Statistical Techniques in Flame Photometry ...... 7 1.1 9 Instrumentation for Analytical Biochemistry ...... 7

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1.20 Computer-Assisted Analytical Chemistry ...... 8 Q 1.21 Analytical Applications of a Digital Instrument Computer System ...... 8 1.21.a Capabilities ...... 8 1.21 .b Planned Use with Special Interfaces ...... 9 . 1.21.c Use as a Laboratory Test Instrument ...... 9 1.21 .d Use for Digital Polarography ...... 9 1.22 Information Packages Submitted to the Division of Technical Information Extension ...... 9 1.23 Cooperative Projects ...... 10

2 . ANALYTICAL METHODOLOGY ...... 11 2.1 GasChromatography ...... 11 2.1.a Instrumentation ...... 11 2.1 .0 A Remodeled Laboratory for Gas Chromatography ...... 11 2.1 .c Device for Sampling Gases Contained in Sealed Metal Tubes ...... 11 2.1 .d Biomedical Applications ...... 12 2.1.e Determination of the Methyl Esters of Butyl Phosphoric Acids ...... 12 2.1 .f Determination of Perfluoromethylcyclohexane in Methane ...... 12 2.14 Preparative Gas Chromatography ...... 13 2.1 .h Derivative Gas Chromatography ...... 13 2.2 Thin-Layer Chromatography ...... 13 2.2.a Instrumentation ...... 13 2.2.b Polytetrafluoroethylene (Teflon) as an Adsorbent ...... 14 2.2.c Constituents of Transfer Ribonucleic Acid (tRNA) ...... 14 2.2.d Amanita Toxins ...... 14 2.2.e Steroids ...... 14 2.2.f Mass Spectrometry of Substances Isolated by Thin-Layer Chromatography ...... 15 2.24 Infrared Spectrometry of Substances Isolated by Thin-Layer Chromatography ...... 16 2.3 Characterization of Tobacco Smoke and Smoke Condensates ...... 16 2.3.a Exploratory Studies ...... 16 2.3.b Thin-Layer Chromatography ...... 16 2.4 Analysis of Water Systems ...... 17 2.4.a Aqueous-Injection Gas Chromatography ...... 17 2.4.b Eutrophic Water Systems ...... 17 2.4.c Deaeration Systems ...... 17 2.4.d Fluorometric Determination of Phosphate ...... 18 2.5 Separation and Concentration Studies ...... 18 2.5.a Column Chromatography with Pentoxide ...... 18 2.5.b Evaluation of a Lipophilic Adsorption Resin for Desalting and Removing Organic Compounds from Water ...... 18 2.5.c Device for the Unattended Concentration of Solutions ...... 19 2.5.d Concentrating ...... 19 2.6 AirQualitySurvey ...... 19 2.7 Research and Support Activities in the Transuranium Research Laboratory ...... 20 . 2.7.a Controlled-Potential Coulometric Determination of ...... 20 2.7.b Titrimetric Determination of Americium ...... 20 2.7.c Micro Titration of ...... 20 2.7.d Voltametric Studies of Plutonium, , and Americium ...... 20 0' vii

2.7.e Modification and Installation of Perkin-Elmer Model 240 Elemental Analyzer in a Glove Box ...... 21 2.7.f Separation of Californium ...... 21 2.7.g Preparation and Analysis of the 0-Diketones of the Lanthanides andActinides ...... 21 2.7.h Purification of 241Amand 243Am ...... 21 2.7.i Spectrophotometric Determination of Plutonium ...... 22 2.8 Polarographic Studies with the Teflon Dropping-Mercury Electrode (D.M.E.) ...... 22 2.8.a Evaluation of Vertical-Orifice Rapid Teflon D.M.E.’s for Obtaining Fundamental Polarographic Data ...... 22 2.8.b Rapid Polarography of in 1 M Hydrofluoric Acid with a Vertical-Orifice Teflon Dropping-Mercury Electrode ...... 22 2.8.c Polarography of Dioxide (Sulfite) in Aqueous Hydrofluoric Acid ...... 22 2.9 Evaluation of the Performance of Ion-Selective Electrodes ...... 23

ANALYTICAL CHEMISTRY FOR REACTOR PROJECTS ...... 23 . J33.1 Molten-Salt Reactor Experiment ...... 23 3.1 .a Determination of in MSRE Salts by Hydrofluorination ...... 23 3.1 .b Determination of Uranium(II1) in Radioactive MSRE Fuel by Reduction ...... 25 3.1 .c Determination of Total Reducing Power of Radioactive MSRE Salts ...... 26 3.1 .d Analysis of MSRE Helium for Hydrocarbons ...... 27 3.2 Analytical Methods for the In-Line Analysis of Molten Fluoride Salts ...... 28 3.2.a Disproportionation of Electrochemically Generated Uranium(V) in Molten LiF-BeF2 -ZrF4 at 500°C ...... 28 3.2.b Voltammetry of (l1) in Molten LiF-BeF2-ZrF4 at 500°C ...... 28 3.2.c Electromotive Force (EMF) Measurements in Molten Fluorides ...... 28 3.2.d Facility for Spectrophotometry of Radioactive Samples ...... 29 3.2.e Spectral Studies of Uranium(V) and Uranium(VI) in Molten LizBeF4 ...... 30 3.2.f Containers for Molten Fluoride Salts ...... 31 3.2.g Absorption Spectra of Several 3d Transition-Metal Ions in Molten Fluoride Solution ...... 31 3.2.h Spectrum of MoF3 in Liz BeF, ...... 31 3.2.i Simultaneous Electrochemical and Spectrophotometric Study of Solutes in Molten Fluoride Salts ...... 32 3.3 Nuclearsafety ...... 32 3.3.a Analysis of Purge Gas from In-Reactor Tests of Reactor Fuel Elements ...... 32

4 . ANALYTICAL BIOCHEMISTRY ...... 33 J 4.1 Macromolecular Separations Program ...... 33 4.1 .a Determination of Tyrosine-Accepting Transfer Ribonucleic Acid (tRNAfYr) ...... 33 4.1 .b Determination of Methionine-Accepting Transfer Ribonucleic Acid (tRNAmet) ...... 34 4.1 .c A Fractional Factorial Method for Optimizing Conditions for the Determination of Transfer Ribonucleic Acid (tRNA) ...... 34 4.1 .d Automated Determination of Transfer Ribonucleic Acids (tRNA’s) ...... 34 4.1 .e Computer Processing of Liquid-Scintillation-Counting Data in the Analysis of Transfer Ribonucleic Acids (tRNA’s) ...... 34 4.1 .f Kinetics of Aminoacylation of Transfer Ribonucleic Acid (tRNA) ...... 35 ... Vlll

4.1 .g Reclaiming Amino Acids-' C ...... 36 0 4.1 .h Chemical Analysis of Transfer Ribonucleic Acids (tRNA's) ...... 37 4.1 .i Terminal Nucleoside Assay of Ribonucleic Acid by Ligand-Exchange Chromatography ...... 38 4.1 .j Gel Electrophoresis of Ribonucleic Acid (RNA) ...... 38 4.1 .k Determination of L-Asparaginase ...... 39 4.1 .1 Determination of Subnanomole Quantities of L-Amino Acids by Isotope Dilution-Aminoacylation ...... 39 4.2 Ligand-Exchange Chromatography ...... 40 4.2.a Principles of Ligand-Exchange Chromatography on -Loaded Chelex Resincolumns ...... 40 4.2.b Separation of Compounds of Biological Interest by Ligand-Exchange Chromatography ...... 41 4.3 Molecular Anatomy Program ...... 41 4.3.a Identification of Urinary Constituents Isolated by Anion-Exchange Chromatography ...... 41 4.3.b Anion-Exchange Chromatography of Hydrolyzed Urine ...... 46 4.3.c Fractionation of Urine by Gel and Anion-Exchange Chromatography ...... 47 4.3.d Gas Chromatographic Analysis of Fractions from the Anion-Exchange Chromatography of Urine ...... 50 4.3.e Desalting of Fractions from the Anion-Exchange Chromatography of Urine ...... 50 4.3.f Gel Electrophoresis of Proteins ...... 51 4.3.g Centriphoresis ...... 51 4.3.h Amino Acid Sequence of Mouse Hemoglobin ...... 51 4.3.i Amino Acid Substitutions ...... 52 4.4 Assistance to Others ...... 52 5 . X-RAY AND OPTICAL SPECTROCHEMISTRY ...... 53 5.1 X-Ray Spectroscopy ...... 53 5.2 Beam Splitter for Use in Calibrating Spectrograpluc Emulsions ...... 53 5.3 Chemical Preconcentration of Trace Elements in Bone Ash ...... 53 5.3.a Reagent Purification ...... 53 5.3.b Removal of Phosphate ...... 54 5.3.c Possible Loss of Cesium During Ashing of Bone ...... 55 5.4 Miscellaneous Trace Determinations Involving Chemical Preconcentration ...... 55 5.4.a Determination of Traces of Rare-Earth Elements in (Carrier-Free Procedure) ...... 55 5.4.b Determination of in Plutonium ...... 55 5.4.c Determination of Traces of Bismuth in LiF-BeF2 Mixtures ...... 55

5.5 Determination of in Curium Oxide (244 Cm203) ...... 55 5.5.a Previous Status of Problem ...... 55 5.5.b NewMethod ...... 56 5.5.c Recovery of Silicon ...... 56 5.5.d Blanks ...... 56 5.5.e Radioactive Contaminants ...... 56 . 6. MASS SPECTROMETRY ...... 57 6 .I Spark-Source Mass Spectrometry ...... 57 6.2 Low-Resolution Mass Spectrometry of Organic Compounds ...... 57

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6.3 Surface Ionization Studies ...... 57 6.3.a Surface Ionization of UF4 at Various Pressures ...... 57 6.3.b Ionization-Potential Measurements ...... 58 6.4 Mass Spectrometric Data Reduction ...... 58 i 7 . OPTICAL AND ELECTRON MICROSCOPY ...... 59 7.1 Research Assistance in Electron Microscopy and Electron Diffraction ...... 59 ' 7.1.a Lanthanide Hydroxide Sols ...... 59 7.1.b Studies of Absolute Filters ...... 60 7.1 .c Studies of Varcum ...... 60 7.1 .d Other Research Assistance ...... 60 7.2 Electron Microscopy of Radioactive Materials ...... 61 7.3 Instrumentation ...... 61

8. NUCLEAR AND RADIOCHEMISTRY ...... 62 8.1 Activation Analysis ...... 62 8.1 .a Air-Floating Sphere for Homogeneous Photon and Neutron Irradiation in Remote Facilities of Uneven ...... 62 8.1.b Photon and Fast-Neutron Activation Analysis at The Oak Ridge Electron Linear Accelerator (ORELA) ...... 62 8.1 .c Neutron Activation Analysis with a 25 Cf Source ...... 63 8.1 .d Influence of Channeling in Customary 3He Activation Analysis ...... 64 8.1 .e Trace Elements in Drugs ...... 66 8.1 .f Neutron Activation Analysis of Brain Tissue for Copper and ...... 66 8.2 New Instruments and Techniques ...... 67 8.2.a Analytical Applications of Cerenkov Radiation ...... 67 8.2.b Photovoltaic Conversion of Radioisotope-Decay Energy ...... 67 8.2.c Alpha-Radiation Damage in Inorganic Phosphors ...... 68 8.2.d Quantitative Electrodeposition of Actinides from Dimethyl Sulfoxide ...... 68 8.2.e A Study of Parameters That Affect Analytical Alpha Spectrometry ...... 68 8.2.f Low-Level Beta Detector ...... 68 8.2.g Liquid-Scintillation Counting of Weak-Beta Emitters in Aqueous Solution by Use of Triton X-100 in an Organic System ...... 68 8.2.h Low-Level-Radiation Counting Facility for Geochemical and Returned LunarSamples ...... 69 8.3 Nuclear Properties of ...... 71 8.3.a Interlaboratory Comparison of Measurements of the Radionuclides 57Co,99Mo-99mTc, and 99mTc ...... 71 8.3.b New Nuclear Data ...... 71 8.3.c Applications of a Be-Window Ge(Li) Spectrometer System ...... 72 8.3.d Nuclear Spectroscopy in the Neutron-Deficient 173 and Fluorine in Molten-Salt-Reactor Graphite ...... 74 8.4.c Measurement by Ge(Li) Gamma Spectrometry of Fission Products Deposited in Components of the MSRE ...... 74 X

A 8.4.d In-Reactor Penetration of Fission Products into MSRE and Pyrolytic Graphite ...... 74 8.4.e Ge(Li) Diode Gamma-Spectrometry System ...... 75 8.4.f Fission-Product Release from Reactor-Fuel Microspheres ...... 75 8.5 14-MeV Neutron Generator ...... 75 8.5.a 14-MeV Neutron Generator Studies ...... 75 8.5.b Determination of Fluorine in Fluorspar by 14-MeV Neutron Activation Analysis ...... 76 8.5.c Neutron Generator Target-Development Program ...... 76 8.5.d 14-MeV Neutron Reaction Research ...... 76 8.6 Cooperative Isotopes Program ...... 76 8.6.a Technical Assistance ...... 76 8.6.b Quality Control ...... 76 8.6.c Radioactivity Standards ...... 77 8.6.d Characterization of Isotope Materials ...... 78 8.6.e Half-Life Measurements ...... 79 8.6.f Production of 1231 for Medical Applications ...... 79 8.64 Special Analytical Assistance for Isotopes Development Center Activities ...... 80 8.6.h Radionuclides in High-Flux Isotope Reactor Coolant Water ...... 80 8.7 Effects of Radiation on Analytical Methods ...... 80 8.7.a Radiolysis of Radiation-Safeguard Spray Solutions ...... 80 8.7.b Radiolysis of Nitrate Solutions ...... 81 8.7.c Radiolysis of Perchloric Acid ...... 82 8.7.d Stability of Some Inert Metals in Irradiated Mineral Acids ...... 82 8.7.e Effect of Radiation on Common Analytical Reagents ...... 83 8.7.f Effect of Gamma Radiation on Spectrophotometric Methods for ...... 83 8.7.g Studies Related to Project Salt Vault ...... 83

1. 9. INORGANIC PREPARATIONS ...... a ...... 84 I J PART B . SERVICE ANALYSES

10. METHODS DEVELOPMENT AND EVALUATION ...... 86 /,I 10.1 New Method for the Rapid Separation of (1V) from (1V) by Anion Exchange ...... 86

10.2 Chromatographic-Solvent Extraction Isolation of 49 Bk from Highly Radioactive Solutions and Its Determination by Beta Counting ...... 86 10.3 New Extraction Chromatographic Method for the Rapid Separation of Americium from Other Transuranium Elements ...... 86 10.4 Thermogravimetric Analysis of Iodate ...... 86 10.5 Gravimetric Determination of Tetrduoroborate with Nitron ...... 87 10.6 Determination of Fluoride in a Mixture of Fluorides ...... 87 10.7 Determination of and Zirconium in Hafnium Oxide-Zirconium Oxide Mixtures ...... 87 10.8 Biochemical Analyses ...... 87 10.9 Rapid-Scan Polarographic Determination of Uranium ...... 87 10.10 Thin-Film Mercury Electrode Voltammetry of Bismuth ...... 88

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A

10.1 1 Characterization of Tobacco Smoke and Smoke Condensates ...... 88 10.1 1.a Literature Survey ...... 88 10.1 1.b ORNL Smoking Machine ...... 88 10.1 1.c Gel-Permeation Chromatography as a Separations Technique ...... 89 10.1 2 Absorption Spectrophotometry of Alpha-Emitting Materials ...... 89 . 10.13 Modified Willard-Winter Distillation Method for Fluoride ...... 89 10.14 Precise Determination of Uranium in MSRE Fuel ...... 89 '11 . SPECTROMETRY ...... 91 11.1 Mass Spectrometry ...... 91 1 1.1 .a Transuranium Mass Spectrometry ...... 91 1l.l.b Mass Spectrometry Services ...... 91 11.2 Emission Spectrometry (Y-12) ...... 91 11.3 Infrared Spectrometry ...... 92 11.4 Nuclear Magnetic Resonance Spectrometry ...... 92 12. PROCESS ANALYSES ...... 94 12.1 High-Level Alpha Radiation Laboratory ...... 94 12.2 General Analyses Laboratory ...... 94 12.3 General Hot-Analyses Laboratory ...... 95 12.4 Radioisotopes-Radiochemistry Laboratory ...... 95 12.5 Radiation Control and Safety ...... 96 12.6 Quality Control ...... 96

PART C. ORNL MASTER ANALYTICAL MANUAL

13. ORNL MASTER ANALYTICAL MANUAL ...... 98 13.1 Cumulative Indexes to the ORNL Master Analytical Manual ...... 98 13.2 Maintenance of the OWLMaster Analytical Manual ...... 98

PART D . ACTIVITIES RELATED TO EDUCATIONAL INSTITUTIONS

14. ACTIVITIES RELATED TO EDUCATIONAL INSTITUTIONS ...... 99 14.1 Advisory Committee Members and Consultants ...... 99 14.2 ORAU Research Participants ...... 99 14.3 Graduate Thesis Research Programs ...... 100 14.3.a ORAU Graduate Fellowship Program ...... 100 14.4 ORNLLoanees ...... 100 14.5 Summer Student Programs ...... 100 14.5.a ORAU Student Trainee Program ...... 100 14.5.b ORNL Undergraduate Program ...... 101 14.6 Alien Guests in Residency ...... 101 xi i

PA RT E. EXT RAL AB0 RAT0R Y PROF ESS I ON AL ACT1VI T I ES

PRESENTATION OF RESEARCH RESULTS Publications ...... 106 Book ...... 106 Contributions to Books ...... 106 Thesis ...... 106 Articles ...... 107 Reports ...... 109 Methods Issued to the ORNL Master Analytical Manual ...... 110 NewMethods ...... 110 FormalIssues ...... 110 Record-Copy Issues ...... 111 RevisedMethods ...... 111 Oral Presentations ...... 111 At Meetings of Professional Societies. Conferences. and the Like ...... 111 Under the Traveling Lecture Program ...... 114 Patents ...... 114

TRANS LAT I ONS

ARTICLES REVIEWED OR REFEREED FOR PERIODICALS

INDEXES KeyWordIndex ...... 119 AuthorIndex ...... 141

ORGAN I ZATl ON CHART Summary

PART A. ANALYTICAL RESEARCH of the Australian Atomic Energy Commission. The polarography of zirconium in acetonitrile and dimethyl 1. Analytical Instrumentation sulfoxide is being investigated in a cooperative study The design work of the Analytical Instrumentation at the Lucas Heights laboratory. Group was continued with stress on operational-ampli- Work in flame photometry was continued with the fier modules and increasing emphasis on digital elec- assembly of a model IX flame spectrophotometer to replace an older model Q-1457 instrument in the hot tronic techniques. Considerable time was devoted to laboratories of the Radioisotopes-Radiochemistry Lab- modifying and upgrading several of the field instru- oratory. A paper that describes signal/noise enhance- ments, to writing new and revising existing methods for ment in flame photometry by statistical techniques is the ORNL Master Analytical Manual, assembling CAPE being prepared. packages, and preparing technical articles for outside For the analysis of tRNA's, a second-generation publication. A substantial number of cooperative ef- automatic sampler was developed. This instrument uses forts were undertaken that involved several projects and electrical synchronization and proper phasing instead of groups - both within and outside the Division. the earlier photometric sensing. A new titrant-delivery The prototype of a modular solid-state coulometric unit and elevator (Q- 1728A potentiometric titrator) titrator in the NIM system will be fabricated for and a new ORNL model Q-1348C servo-pipetter were ultimate replacement of the older Q-2005-X50 instru- fabricated in the ORNL machine shops for the High- ments that have seen as much as ten years of contin- uous laboratory service. Optimum and compatible Radiation-Level Analytical Laboratory. electrochemical cell design is aimed at shorter titration Operational amplifiers were used in an instrument for times and the achievement of accuracy and precision on end-point detection in bipotentiometric titrations and smaller amounts (

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develop. Consequently, the activities of this group are ration and found that the air in the Eagle Bend very diverse and often supplement the efforts of other Industrial Park is of typical nonurban quality. groups. For example, a new research-quality gas chro- Our activities in the Transuranium Research Labora- matograph was acquired for use by both the Analytical tory (TRL) involve both analytical research and general Biochemistry and the Analytical Methodology Groups. chemical support. We have conducted several electro- We have initiated programs of study in biomedical analytical studies of the lighter transuraniums. With applications of gas chromatography (GC), in derivative these elements, precise analytical methods are needed GC, and in aqueous-injection GC. Other GC develop- so that their fundamental characteristics can be better ments include a method for determining perfluoro- determined. We hope ultimately to use thin-layer methylcyclohexane in methane, resolution of the electrochemical techniques to study these elements. methyl esters of the phosphoric acids that derive from Considerable assistance of both an analytical and a degradation of tributyl phosphate, and the purification preparative nature has been given to many members of of some 16 compounds by preparative GC. A labora- the TRL staff. tory has been remodeled specifically for gas chromato- graphic work. 3. Analytical Chemistry for Reactor Projects Means for concentrating, desalting, and separating materials, especially tiny amounts of organic materials, Oxide concentrations in the MSRE fuel, as deter- are needed to an increasing extent. We have continued mined by the hydrofluorination method, remained near our work in thin-layer chromatography. Several fruitful the 50-ppm level. The essentially identical result ob- applications of TLC have been made, and we are tained in the analysis of a sample maintained at an currently evaluating its utility when conjoined with elevated temperature to minimize radiolysis virtually other analytical techniques, such as mass and infrared proved that the radioactivity of the samples does not spectroscopy. We anticipate studies in quantitative TLC produce a negative bias in the results. Oxide was also and have acquired an instrument for such studies. The determined on LiF-BeF2 preparations and on samples lipophilic resin Amberlite XAD-2 has been explored as a of LiF-UF4 from the production of 233Ufuel concen- means for collecting and/or desalting solutions of trates. These latter samples required the development of organic materials. We anticipate a continuing program new sampling techniques and the adaptation of the of study, evaluation, and application of techniques and method to smaller samples and to new forms of sample materials for isolation of organic compounds. containers. An evaluation of the operating history of We are participating, along with several other mem- the hot-cell apparatus for oxide determination indicated bers of the Division, in a new program to develop an that electrolytic moisture-monitor cells are desensitized analytical scheme for characterizing tobacco smoke and rapidly during the analysis of highly radioactive sam- smoke condensates. Our efforts in this program have ples; however, similar desensitization of a test cell could been largely exploratory to date, with emphasis on not be produced by exposure to radioactivity of fractionation and separation of the multitudinous com- comparable and higher levels. All current and previous \ pounds into classes. Gas-liquid and thin-layer chroma- results of the determinations of the U3+/U4' ratio in the tography will be used extensively in this program. MSRE fuel were reevaluated by means of a modified Our efforts in water analysis fall broadly into two computer program that calculates ratios at the opera- areas: analysis of deaerated and saline waters and ting temperature of the reactor rather than at the lower analysis of waters of ecological significance. Efforts to temperatures at which the analyses were performed. improve the methods used to determine oxygen in very With the exception of three results, apparently associ- low concentrations in water have continued, because ated with samples of the highest radioactivity, the such methods are needed to calibrate and evaluate any recomputed ratios are in reasonable agreement with the instrumental method that may be considered. We have ratios calculated on the basis of the operating history of evaluated several instrumental methods and have con- the reactor (i.e., additions, corrosion-product tinued to provide on-site analytical support for tests of increases, and allowance for burnup). A method for the several desalination plants. The new aqueous-injection remote measurement of traces of HF in gas streams has gas chromatography project mentioned above offers been developed to cover the range of concentrations (8 considerable promise for analysis of waters of ecological to 400 ppm) found in hydrogen-transpiration effluents. importance. The method is based on the preconcentration of the HF We conducted a brief air-quality survey for the on an NaF trap and thermal-conductivity measurement neighboring Melton Hill Regional Development Corpo- of the pulse of HF generated on desorption. The XV

hydrogen-evolution method, which is a measure of both 4. Analytical Biochemistry U(II1) and dispersed electropositive metals, is being modified for adaptation to radioactive samples of Analytical assistance to the Biology and Chemical reprocessed MSRE fuel solvent. To avoid loss of Technology Divisions was continued in support of the reducing power of samples during pulverizations, sam- Macromolecular Separations and Molecular Anatomy ple fragments are dissolved in HC1-HBO3 at 250°C in a Programs. In the analysis of transfer ribonucleic acids sealed tube. An in-line analyzer that was installed to (tRNA’s), the optimum conditions for the assay of measure traces of hydrocarbons in the MSRE off-gas tyrosine- and methionine-accepting tRNA’s were estab- was found to be subject to substantial radiation lished, and a statistically designed program for optimi- interference. This interference was determined to be zation studies is now being used. Our automated caused by radiolysis of moisture on the reagents used to analyzer has been modified to operate more economi- absorb the combustion products of hydrocarbons and cally, and a technique for recovering C-labeled amino will be minimized by the substitution of a small acids was developed. The raw assay data are now being regenerable molecular-sieve trap. processed by computer; the processed data are pre- sented as both a tabulation and a plot. Studies of the The electrochemical oxidation of U(1V) in molten kinetics of aminoacylation are continuing to provide a LiF-BeF2 -ZrF4 has been studied. Experimental evi- better understanding of the assay. Methods for deter- dence indicates that the U(V), which is formed, mining impurities in tRNA have been improved. Future subsequently disproportionates into U(IV) and U(VI). plans for the Macromolecular Separations Program Also, the electrochemical reduction of Cr(I1) in this include separations of ribosomal RNA and various same solvent was studied by conventional and first- enzymes; consequently, we are developing methods to derivative voltammetry. Although U(IV) interferes to measure high-molecular-weight RNA by gel electro- some extent, it is believed that the Cr(I1) + Cr(0) phoresis and are investigating the assay of the enzyme reduction wave can be used to monitor chromium in L-asparaginase. As a “spinoff’ of this program, we find fluoride melts. The emfs of several metal-metal ion that the aminoacylation reaction can be used in an couples vs an Ni/Ni(II) reference electrode were meas- ultrasensitive isotope-dilution method for the determi- ured in molten fluorides at 500°C. Because nation of L-amino acids. nitride does not appear to be entirely satisfactory as a Further research into the principles and applications sheath for the reference electrode, it is planned to of ligand-exchange chromatography is being carried out. investigate the use of metal frits for separating the For the Body Fluids Analysis Group of the Molecular reference electrode from the bulk of the melt. Anatomy Program, we are attempting to isolate and The designing of the in-cell equipment of a fachty for characterize compounds separated from urine by spectral studies of highly radioactive materials is essen- anion-exchange chromatography. Two compounds were tially complete, and some of these components are now identified definitely and several others tentatively. being fabricated. This equipment will permit the trans- Conjugates of various types were located from chro- fer of samples of radioactive fluoride salts to spectro- matograms by chromatography before and after enzy- photometric cells without exposure of the samples to matic or acid hydrolysis. Prefractionation of urine by the atmosphere and will simultaneously maintain them gel chromatography into six fractions followed by at a temperature sufficient to eliminate significant anion-exchange chromatography of the individual frac- radiolysis. A diamond-windowed cell has been devel- tions improves the purity of the compounds isolated. oped for use with molten fluoride salts. We will also attempt the gas chromatographic analysis The study of the spectra of Fe(II), Ni(II), Cr(II), and of fractions from anion-exchange chromatography after Cr(II1) in various LiF-BeFz melts has been concluded. extraction or forming derivatives in the desalted and Studies of the spectra of U(V), U(VI), U022+,and lyophilized material. Mo(II1) have been initiated or continued. Solvent Gel electrophoresis and centriphoresis were used to contaminants, primarily products of hydrolysis, have concentrate and isolate tumor antigen activity and to been found to greatly affect the electrochemical genera- separate other large proteins. Amino acid sequence tion of solute species for spectral characterization. analysis of mouse hemoglobins was continued. Con- Vacuum pretreatment of LiF-NaF-KF at 450°C is sideration of the frequency of certain substitutions in effective in removing the HzO precursor. The electro- the j3 chain led to the conclusion that gene duplication chemical generation of and copper in their is the primary cause of chain heterogeneity. Amino acid various oxidation states for spectral study is presently analyses were also done for several members of the being investigated. Biology Division. xvi

5. X-Ray and Optical Spectrochemistry Between -1500" and -2250"K, the effects of com- peting reactions hinder satisfactory interpretation of A code has been written for converting x-ray diffrac- the data. A measurement of the ionization potential of tion data to lattice parameters. A technique has been thorium has yielded a tentative value of 7.5 2 0.3 eV. developed for determining sulfur-to- ratios in small organic samples with the electron probe. The 7. Optical and Electron Microscopy optical and mechanical design of a beam splitter for calibrating spectrographic film has been optimized, and Optical and electron microscopy and electron diffrac- the best conditions for its use were determined for tion have been applied to many problems arising in different types of spectrographs. Preconcentration pro- fundamental and applied research. These include studies cedures were devised for traces of rare-earth elements in of lanthanide hydroxide sols and absolute filters at bismuth, cadmium in plutonium, and bismuth in elevated temperatures and the characterization of LiF-BeF2 . In the electrodialysis-Mitchell-Scott proce- "good" and "bad" Varcum, which is a furfuryl alcohol dure for determining trace elements in bone, the derivative. Observations of radioactive materials have removal of phosphate was accelerated by use of a continued in connection with a NASA project and with two-compartment electrodialysis cell. Recoveries and the MSRE. An electron-beam vaporizer is being used to total process blanks were determined for numerous produce ultrapure thin films. The "hot" microscope in trace impurities. A procedure was developed for deter- Building 3019 is being replaced with a newer model, mining silicon in curium oxide. and the Philips EM 300 electron microscope is being installed in the Transuranium Processing Plant. 6. Mass Spectrometry 8. Nuclear and Radiochemistry A trace characterization analysis of 242Pu (tlp = An air-floating sphere for homogeneous photon and 3.79 X 10' y) was conducted by use of the solution neutron irradiations in nonuniform neutron-flux envi- spark-source technique. Twenty-one genera1 contami- nants were found. The distribution of rare-earth ele- ronments was designed for use in the ORELA. Cross sections for activation-analysis experiments with a ments in different leaf and wood ash samples was determined. 2'2Cf source were measured by use of an 0.87-mg source. Investigation of He activation analysis con- The low-resolution mass spectrometer has been used tinued with the study of channeling effects. Among the to record the spectra of a wide variety of organic applied activation-analysis programs are two coopera- compounds for identification or elucidation of struc- tive efforts: trace elements in drugs (with the Bureau of ture and to accumulate reference spectra for known Drug Abuse Control) and copper and manganese in compounds. For samples of adequate size and purity, brain tissue (with ORAU). the mass spectrometry has been coordinated with Preliminary studies of the use of Cerenkov radiation nuclear magnetic resonance and infrared spectrometry. for measurement and the study of alpha All three of these techniques have been applied with damage in inorganic phosphors were begun. The investi- some success to service problems for ORNL and Y-12. gation of photovoltaic conversion of radioisotope decay The analytical effort has been slanted toward support energy was completed. Actinide electrodeposition from of the Body Fluids Analyses Program. The difficulty so dimethyl sulfoxide for preparation of alpha-counting far has been that the samples available are small and sources and the variables that affect alpha spectrometry frequently of dubious purity. Informal sessions on were studied. Counting of weak-beta emitters in an techniques have been held at approximately monthly aqueous solution was improved through use of Triton intervals to bring together Division personnel involved X-100, and the low-level-radiation counting facility at in the bioanalytical work and to keep them informed Houston for returned lunar samples was completed and on techniques and results. equipment was installed in it. Surface ionization studies have shown that, in the Interlaboratory comparison of measurements of the presence of oxygen, the emission of U02+ from nuclides "Co, "Mo-'~~Tc, and 99mTc was made. filaments exhibits two maxima as the tempera- Among new nuclear data reported are energies of ture is increased. The temperatures at which these gamma rays in C1 and ' ' In, cross sections for Ni maxima occur are very weakly dependent on the partial and '08Pb, gamma branchings and conversion coeffi- , pressure of oxygen. Below -1 500"K, the evaporation cients in ' Pd-' Rh, and gamma-ray intensities in energy of UOz+ is deduced to be -6.9 k 0.4 eV. the decay of ' Ba. By use of a thin-window Ge(Li) xvii

A detector, the 53-keV gamma ray of 73Aswas measured were the preparations of ferrites (Fe304-type com- in the presence of other radioisotopes; this pounds) and some high-purity fluorides, the purifi- detector has been calibrated for efficiency. The investi- cation of MgO, and the heat treatment of rare-earth- gation of nuclear properties of neutron-deficient rare- metal alloys. The production of 50 g of 16'Gd was earth elements continued with studies in the 173 < A < accomplished. For the Physics Division, numerous AuLi 185 region. alloys were prepared and also some isotopic intermetal- Considerable effort was spent in applying nuclear lic compounds that contain Ni, Ni, and l3Ge. The methods to reactor program problems. Delayed-neutron decontamination of -7 kg of platinum was undertaken counting made possible a highly precise U determi- for the Stores Department. nation. The 3-MeV Van de Graaff generator was used to determine lithium and fluorine in MSRE graphite, and a PART B. SERVICE ANALYSES highly collimated Ge(Li) spectrometer was used to The Methods Development and Evaluation Group was determine deposited fission products in the MSRE heat united with the Service groups this past year, and the exchanger. In addition, in-reactor fission-product pene- union of these groups has worked out very satisfac- tration of specimen graphite was determined by torily. gamma-ray spectrometry. A IO-cc Ge(Li) detector was set up to assist in measuring fission-product release 10. Methods Development and Evaluation from reactor-fuel microspheres. The 14-MeV neutron generator has been used to determine oxygen in a Several new radiochemical methods have been devel- variety of materials and fluorine in fluorspar and to oped; they include the anion separation of Bk(IV) from evaluate the usefulness of new targets. In addition, a Ce(IV), isolation of Bk by solvent extraction and its new target into which tritium continuously diffuses has determination by beta counting, and separation of been designed. Both the Texas Nuclear Corporation and americium from other transuranium elements by extrac- the Kaman machines have been used by a number of tion chromatography. extradivision experimenters. A variety of special work included the thermogravi- Quality control for products of the Isotopes Division metric analysis of thorium iodate, gravimetric determi- continued as an important assistance, as did checking of nation of tetrafluoroborate, determination of fluoride commercially available radioactivity standards used in molybdenum fluoride, and determination of hafnium thsrein. Data have been evaluated and, in some in- and zirconium in their mixed . stances, measurements made for inclusion in the Iso- Two of the newer electroanalytical methods were topes Users' Guide; for example, half-life values for 36 evaluated for special applications: rapid-scan derivative radionuclides were published. Techniques were devel- polarography for determining uranium in synthetic oped for production of 1231 for medical purposes. MSRE fuel and thin-film mercury-electrode voltam- Study of radionuclides in HFIR coolant water was metry for bismuth. continued. A literature survey was made for the Smoking and Health Program, A smoking machine was fabricated and Jnvestigation of the radiolysis of radiation-safeguard used to collect cigarette-smoke condensates. The com- spray solutions continued as a contribution to spray ponents of tobacco extracts were separated by gel- and absorption technology. The radiolysis of nitrate solutions and of perchloric acid solutions and the permeation chromatography. stability of some inert metals in irradiated mineral acids The work in absorption spectrophotometry of alpha- also received attention. A chapter concerned with effect emitting materials has continued. of radiation on common analytical reagents was pre- Uranium was separated from radioactive MSRE fuel pared for a book, and the effect of gamma radiation on by fluorination in a shielded hot cell. The resulting uF6 spectrophotometric methods for iron was studied. The was absorbed in a fluoride trap, dissolved in effect of moisture in the salt beds of interest in Project sulfuric acid, and determined by controlled-potential Salt Vault was evaluated. coulometric titration at a relative standard deviation of 0.1%. 9. Inorganic Preparations 11. Spectrometry

The preparation of fused salts continued but on a In mass spectrometry, the Transuranium Mass Spec- reduced scale and mostly for the Metals and Ceramics trometry Laboratory continued to make isotopic analy- 'A Division. The main activities for the Solid State Division ses for a diverse group of customers. The half-lives of xviii

242Pu and 244Pu were measured, and the new values transuranium process solutions. Oxygen-to-metal ratios were published. Work was also done to measure the were determined on Pu02-U02pellets. A new proce- half-lives of some other transuranium elements. The dure for dissolving high-fired Pu02-U02 was adopted. isotopic analysis of all elements from thorium through The work load of the General Analyses Laboratory einsteinium was done routinely. The total number of increased -35%. A method for bulk- measure- analyses reported by the Mass Spectrometry Service ment of large porous graphite specimens was developed. Laboratory increased 20% over last year. The increase A pycnometer was constructed for measuring the included gas samples and stable and radioactive solid density of 0.1-cc samples. The arsenazo 111 method was samples. used to determine thorium in bismuth metal. The Spectrochemistry Laboratory (Y-12) reported The General Hot-Analyses Laboratory continued the 47,000 results of emission spectrochemical analyses on same type of work as was done last year. Equipment for 2500 samples, which represents increases of 12 and fluorinating uranium from MSRE fuel-salt samples was 19%,respectively. More than 300 bismuth samples from set up for use in a work cell for determining uranium. A the MSRE salt cleanup program were analyzed for Kollmorgen periscope was installed through the cell- thorium, lithium, and beryllium. block wall for visually examining radioactive materials. In the Infrared Laboratory, various samples of or- The Radioisotopes-Radiochemistry Laboratory con- ganic, organometallic, and inorganic nature were exam- tinued to use computer resolution of gamma-ray spec- ined. The information desired is primarily qualitative in trometric data for the divisions requesting radioactive nature and usually involves identification, structure, data. To facilitate the acquisition and processing of changes in structure, and presence of impurities. Oc- radiometric data, a 4096-channel pulse-height analyzer casional quantitative work also was performed. Devel- and an IBM card punch were purchased. Computer opment or modification of instruments or techniques is programs have been written for qualitative and quanti- done when it is pertinent to the service work. tative Ge(Li) spectrometry. In nuclear magnetic resonance (NMR) spectrometry, The Radiation Control and Safety personnel con- the NMR Spectrometry Laboratory rendered support to tinued their work, primarily in Buildings 3019 and several ORNL, Y-12, and ORAU research divisions 2026. In July, construction of the West Annex to through the recording and interpretation of the NMR Building 2026 (HRLAL) was begun. spectra of organic compounds that resulted from The number of control samples included in the studies being carried out in these divisions. Often this Statistical Quality Control Program decreased 22.6%; service was a combined effort of the Mass, Infrared, and the apparent overall quality of the work decreased NMR Laboratories. slightly as a result of the initiation of several new control programs for which the 2S limits have not yet 12. Process Analyses been established.

The laboratories doing process analyses performed PART C. ORNL MASTER 207,100 analyses, which is about the same as the past ANALYTICAL MANUAL year, but we had a 12% decrease in personnel. The largest number of samples came from the Transuranium 13. ORNL Master Analytical Manual Process and biochemical programs. Brief statements Five new methods were added to the Manual; one of about the work and new developments in each labora- these was for the purpose of record only. Revisions tory follow. were made to six methods. The status of nine methods The High-Level Alpha Radiation Laboratory put into for the Transuranium Process was changed from tenta- service a method for the determination of berkelium in tive to formal. Part A. Analytical Research

The research program of the Analytical Chemistry ical research and development is also being conducted Division is indicative of the diversification of the total in several areas of biochemistry and bioengineering for effort in analytical chemistry at the Oak Ridge National the National Institute of General Medical Sciences and Lab oratory . National Cancer Institute of the National Institutes of Investigations in analytical instrumentation, nuclear Health. Programs were continued to provide specific methods of chemical analysis, electroanalytical chem- assistance to research divisions and projects of the Oak istry of molten salts, radiation effects on analytical Ridge National Laboratory, for example, the Molten- methods, and mass spectrometry are carried out for the Salt Reactor Project and Transuranium Process Pro- Division of Research of the Atomic Energy Commis- gram. sion. Studies of applications for radioisotopes are done The progress in these investigations is presented in the for the AEC Division of Isotopes Development. Analyt- following sections.

D. J. Fisher R. W. Stelzner

1.1 SOLID-STATE CONTROLLED-POTENTIAL rent-limiting amplifier. The current module contains the COULOMETRIC TITRATOR current amplifier, current booster, and part of the automatic cutoff circuitry. The meter module contains T. R. Mueller H. C. Jones the current meter, meter-driver amplifier, automatic- The circuit designs and tentative panel layouts of cutoff-detector amplifier, and part of the automatic three of the four modules for the solid-state controlled- cutoff circuitry. A fourth module will house an analog potential coulometric titrator have been completed.’ integrator. The modules will be fabricated by the Instrument Two modes of current integration will be available. Department of the Instrumentation and Controls Divi- One will use a voltage-to-frequency converter followed sion. The potentiostat module contains the reference- by an electronic counter; the other will use an electrode-follower amplifier, control amplifier, and cur- operational amplifier to perform analog integration. For operation, only one mode of integration is needed. However, for I vs Q recordings, the analog integrator ‘H. C. Jones and T. R. Mueller, “Solid-State Controlled- module is required. Potential Coulometric Titrator,” Anal. Chem Div. Ann. Progr. After the first instrument is fabricated, the cell-design Rept. Oct. 31, 1967, ORNL-4196, p. 3. studies will be continued in an effort to decrease

1 significantly the total titration time and to increase the displacement liquid and therefore does not require the precision and accuracy of the titration of samples that higher corrosion resistance of the usual Graphitar contain <1 mg of the substance to be determined. plungers. Check-out of the pipetter was completed. For it, a pipet that has a displaceable volume of 3.0 ml(l.0 1.2 MODIFICATIONS TO THE HIGH-SENSITIVITY ml is standard) was built and is being evaluated. CONTROLLED-POTENTIALCOULOMETRIC TITRATOR (ORNL MODEL Q-2564) 1.4 APPARATUS FOR PRECISE CONTROL OF MERCURY FLOW RATE OF T. R. Mueller D. J. Fisher DROPPING-MERCURY ELECTRODES (D.M.E.’s) H. C. Jones R. W. Stelzner D. J. Fisher W. L. Maddox The five model Q-2564 coulometric titrators2 in use in the Division were modified by the Instrument We are continuing to study the precision attainable in Department of the Instrumentation and Controls Divi- single-cell first-derivative dc polarography.6 For this sion and returned to operation. The modifications have work, a positive-displacement pump was developed to been de~cribed.~>4 deliver mercury at a constant rate through the D.M.E. capillary. A prototype apparatus has been assembled that uses a high-precision Gilmont piston buret con- 1.3 INSTRUMENTATION FOR THE nected to the capillary through an all-glass system. The HIGH-RADIATION-LEVEL capillary is mounted in the model Q-2942 polarographic ANALYTICAL LABORATORY (HRLAL) drop-time controller described earlier.7 The evaluation W. L. Maddox of this assembly is in the preliminary stages. 1.3.a New Titrant-Delivery Unit and Elevator 1.5 ELECTRICAL AND ELECTROCHEMICAL TESTS OF PERFORMANCE OF POLAROGRAPHS A new titrant-delivery unit (TDQ and elevator assembly of the type described previously5 were fab- D. J. Fisher W. L. Belew M. T. Kelley ricated and checked out for use with the automatic The abstract from a paper accepted for publication potentiometric titrator (Q-l728A) in the HRLAL. follows:8 Plexiglas shields, to give increased protection against “Both electrical and electrochemical tests are required in inadvertent spills and mechanical mishandling, were order to define, describe, and specify the performance of a added to the new assembly. The drawings that describe polarograph, when a polarograph or a cell or an electrode is the TDU and elevator were revised to show the new newly constructed or placed in service, when work is to be parts. started that is of special importance, or when poor results are obtained with a combination that has been in use. In the last case, the fist question is whether the malfunction originates in 1.3.b New ORNL Model Q-1348C Pipetter the polarograph itself or in the cell-electrode assembly or is due to electrochemical problems specific to the sample just intre A new OWL model Q-1348C pipetter was fabricated duced. The polarograph is tested by means of electrical tests. If in the ORNL shops. Stainless-steel plungers were made it is performing according to specifications, the overall system for this unit, since it will be used with a secondary

‘W. L. Belew, D. J. Fisher, M. T. Kelley, R. W. Stelzner, and ’H. C. Jones, W. D. Shults, and J. M. Dale, “High-Sensitivity E. S. Wolfe, “Investigation of Precision Attainable in Single-Cell Controlled-Potential Coulometric Titrator,” Anal. Chem 37, First-Derivative DC Polarography,” Anal. Chem. Div. Ann 680 (1965). Progr. Rept. Oct. 31, 1967, ORNL-4196, p. 7. 3T. R. Mueller and H. C. Jones, “Modifications to the 7W. L. Belew, H. C. Jones, D. J. Fisher, and M. T. Kelley, High-Sensitivity Controlled-Potential Coulometric Titrator “Apparatus for Precise Control of Drop Time of a Dropping- (ORNL Model Q-2564),” Anal. Chem Div. Ann. Bog. Rept. Mercury Electrode (D.M.E.) (ORNL Model Q-2942),” Anal. Oct. 31, 1967, ORNL-4196, p. 3. Chem Div. Ann Progr. Rept. Oct. 31, 1967, ORNL-4196, p, 6. 4T. R. Mueller, H. C. Jones, D. J. Fisher, and R. W. Stelzner, 8D. J. Fisher, W. L. Belew, and M. T. Kelley, “Electrical and “Modifications of the ORNL Model Q-2564 High Sensitivity Electrochemical Tests of Performance of Polarographs. I. Needs Coulometric Titrator,” ORNL-TM-2175 (Mar. 18, 1968). and Methods. 11. ‘Diagnostic Criteria for Establishing the Degree ’W, L. Maddox, “Titrant-Delivery Unit and Elevator for the to Which Recorded Polarograms Are Adversely Affected by ORNL Model Q-1728 Potentiometric Titrators,” Anal. Chem. Circuit Performance,” accepted for publication in Chemical Div. Ann Progr. Rept. Oct. 31, 1966, ORNL-4039, p. 6. Instrumentation. 3

8 (and thus the cell and electrodes) is checked out by means of reproducible and the inherently superior resolution for first obtaining polarograms with reactions of well known character- derivative dc polarography is achieved. Because superior signal- istics. Satisfactory electrical and electrochemical test methods to-noise ratio is achieved at faster scan rates, up to 3 v/min, the which have evolved at Oak Ridge National Laboratory (ORNL) first and second derivative dc polarograms obtained at these are set forth in this paper. For any specific polarograph, each of scan rates are more useful when the sensitivity of measurement these tests is generally applicable, provided, of course, that the is of principal interest. Due to the greater ease of measurement polarograph includes the feature or mode of operation for at high sensitivity, rapid second derivative dc polarography is of which the test is designed. Also, diagnostic criteria are given for particular advantage. Such polarograms can be recorded in as establishing the degree to which the forms of recorded regular, little as 10 sec. By using an XY recorder, the X axis is fist derivative, and second derivative dc polarograrns (for independent of scan rate and replicate polarograms are super- simple, polarographically reversible test reactions) are adversely imposed. affected by circuit performance.” “Data is presented showing the ultimate resolution is achieved with first derivative dc polarograms and that the peak-to-peak height of second derivative dc polarograms is linearly related to 1.6 A CONTROLLED-POTENTIAL AND concentration over the range tested, 5 X to 1 X M.” DERIVATIVE DC POLAROGRAPH - ADVANTAGES OF RAPID AND 1.7 POLAROGRAPHY OF ZIRCONIUM DERIVATIVE DC POLAROGRAPHY IN ACETONITRILE AND DIMETHYL SULFOXIDE W.L. Belew T. M. Florence” D. J. Fisher W. L. Belew M. T. Kelley The possibility was investigated of obtaining polarog- The abstract from a paper accepted for publication raphic waves due to the reduction of zirconium species follows:9 to lower valence states in nonaqueous solvents. Re- “The circuits, theory, and performance characteristics are described of a controlled-potential dc polarograph (ORNL duction waves are reported for zirconium in dimethyl model Q-1988-FES) which is designed to take advantage of the sulfoxide (DMSO)’ ’ and in acetonitrile;’ therefore, inherent high sensitivity and resolution of derivative dc polar- preliminary work was done with these compounds as ography. Several circuit modifications for specific applications solvents. are described. Cell and electrode design considerations are given. Since traces of water are expected to greatly affect The advantages of potentiostatic electrolysis in polarography, the advantages of the use of current-averaging and analog waves for a substance in nonaqueous media as easily derivative circuits in improving the measurement and the hydrolyzed as ZrCL, effort was made to ensure at all interpretation of recorded dc polarograms, the attainment of times the lowest possible water content of the support- ultimate high resolution through the recording of first derivative ing media. All solutions were prepared in a dry box. dc polarograms of good wave form, the achievement of high Their water contents were determined by Karl Fischer sensitivity by means of rapid derivatice dc polarography, the practical advantages of fist derivative over regular dc polarog- titration before and after each series of polarograms. raphy, the relative advantages of fist and second derivative dc DMSO with a water content as low as 5 X M was polarography, and the practical advantages of rapid dc polarog- obtained by shaking the DMSO with freshly activated raphy are discussed. Conclusions are illustrated and substanti- Linde type 5A molecular sieve. Acetonitrile with a ated by data. water content of 2 X M was obtained by “With a 2 to 5 sec D.M.E., controlled-potential undamped, fractional distillation from P2 O5 and CaHz maximumcurrent, or averagecurrent regular dc polarograms or . first derivative dc polarograms can be recorded. With a low In DMSO, 0.1 M in tetrapropylammonium perchlo- average mercury flow rate 0.5 sec D.M.E., controlled-potential rate and with a water concentration of 6 X low3Mor rapid averagecurrent regular dc polarograms or first or second greater, two waves for zirconium tetrachloride are derivative dc polarograms can be recorded and instrumental observed. Their E,j2 values are - 1.04 and - 1.60 V vs conditions can be selected that result in optimizing either aqueous S.C.E. The wave at -1.04 V is identical resolution or sensitivity (signal-to-noise ratio). At scan rates up an to 0.3 v/min, the recorded forms of regular and derivative waves agree well with the usual, accepted equations. Under these conditions, regular averagecurrent and first derivative dc “Australian Atomic Energy Commission Research Estab- polarograms are particularly useful, since they are highly lishment, Sutherland, New South Wales, Australia. “G. Schober and V. Gutmann, “Die Polarographie in Wasserfreiem Dimethylsulfoxyd,” pp. 940-47 in Advnnces in ’D. J. Fisher, W. L. Belew, and M. T. Kelley, “A Controlled- Polarography (Proceedings of the Second International Con- Potential and Derivative DC Polarograph for Regular and First gress, Cambridge, 1959), ed. by 1. S. Longmuir, vol. 3, and Second Derivative DC Polarography: Circuits, Theory and Pergamon, London, 1960. Performance Characteristics. Advantages of Rapid and Deriva- ’ J. W. Olver and J. W. Koss, Jr., “Polarography of Zirconium tive DC Polarography,” accepted for publication in Chemical and Hafnium in Acetonitrile,” J. Inorg. NucL Chem 25, 1515 Instrumentation. (1963). 4

with that obtained when only free HC1 is added to the systems (0.1 M sodium acetate and 0.1 M sodium supporting medium, and therefore this wave is believed acetate-0.1 M acetic acid) were chosen to match to be due to free HCI formed by the reaction of ZrCl, conditions in the elution step of chromatographic with water. The wave at -1.60 V is ill-formed and very processes. Gelatin (0.01%) and Triton X-100 (0.001%) irreversible; it is believed to be a “hydrolytic wave,” were used as maximum suppressors when needed. because both the height and the form of the wave The differential subtractive two-cell modes of opera- depend on the water concentration. In DMSO that has a tion were tried with and without sparging and with and water content of <1 X M, ZrC14 appears to be without maximum suppressors. For adequate repro- only slightly soluble. ducibility, sparging and a maximum suppressor were Although three reduction waves had been reported found to be necessary, in addition to careful control of for ZrCt, in acetonitrile (tetraethylammonium perchlo- D.M.E. and cell operation. rate as supporting electrolyte),’ * we observed only one Survey polarograms were run on 23 compounds irreversible wave for ZrCl, in the system acetonitrile- selected from five major groups: pyrimidines, purines, 0.1 M tetrapropylammonium perchlorate-0.1 M water. pyridine derivatives, benzene derivatives, and amino When the water content was reduced to 2 X M, acids. Reduction waves were obtained for ten com- ZrCL appeared to be only slightly soluble. pounds in 0.1 M acetic acid-0.1 M sodium acetate and Even though the ZrC4 is reagent grade (99.9% pure), for eleven compounds in 0.1 M sodium acetate. Only some impurity may be present. Further studies will be three compounds gave clearly defined reduction waves done with reagent-grade ZrCL that has been sublimed. in acid media: pyridoxal, cystine, and uric acid. Reduction waves for all other compounds were associ- 1.8 POLAROGRAPHIC SURVEY ated with the hydrogen-discharge wave. Waves in 0.1 M OF BIOCHEMICALS sodium acetate were better defined but not completely resolved from the hydrogen-discharge wave. Half-wave C. R. Spell’ D. J. Fisher potentials vs S.C.E. were obtained for all waves that were well enough defined for measurement. In the ORNL Body Fluids Analyses Program,’ Nicotinamide and pyridoxal were selected for quanti- biochemicals that are urinary constituents are separated tative study in the acid buffer system with the in high-resolution chromatographic columns. A survey differential subtractive modes. Nicotinamide gives a has been made of the dc polarographic characteristics of reduction wave on the slope of the hydrogen-discharge selected examples of these biochemicals. Also, the wave; pyridoxal gives one somewhat before that slope. feasibilities have been assessed of using dc polarography For the concentrations 0.02,0.04, and 0.08 mg/ml, the to qualitatively and quantitatively monitor column- linearity of response indicates that quantitative estima- effluent streams and for laboratory identification and tion is possible. concentration analyses of biochemicals in column frac- Survey polarograms were run on 5-ml samples col- tions. lected from a chromatographic column. To check the Survey polarograms were obtained with the ORNL feasibility of the polarographic technique as a monitor- controlled-potential differential dc polarograph.’ The ing tool without the addition of either supporting instrument was used in its regular and first-derivative electrolyte or maximum suppressor, the 5-ml samples modes for single-cell operation and its differential were diluted to 50 ml with distilled water and placed in subtractive modes’ for two-cell operation. Buffer the cells. The samples were sparged with argon, and polarograms were recorded by the regular single-cell method; first-derivative curves were obtained on some 30RAU Research Participant; Professor of Chemistry, ’ of the samples. It was discovered that, without addi- Emory and Henry College, Emory, Va. 14C. D. Scott, Progress Report for the Period March I, tional supporting electrolyte, apparent reduction waves 1967-March I, 1968, Body Fluid Analysis Program, ORNL- appeared on the derivative curves. They were not TM-2184 (April 1968). reproducible and were drawn out. This behavior was ”W. D. Shults, D. J. Fisher, H. C. Jones, M. T. Kelley, and W. attributed to migration currents and was checked by B. Schaap, “Controlled-Potential Differential DC Polarography. taking 25 ml of the sample from the polarograpluc cell I. Instrumentation, Apparatus, and Techniques,” Z. Anal. and adding sufficient acetic acid and sodium acetate to Chem 224, l(1967). make the solution 0.1 M with respect to each when 16W. D. Shults, D. J. Fisher, and W. B. Schaap, “Controlled- Potential Differential DC Polarography. V. Subtractive Polar- diluted to 50 ml with distilled water. The solutions so ography,” Chem Instr. 1, 7 (1968). prepared contained the equivalent of 2.5 ml of the a’ 5

0 original sample. Polarograms were again recorded; in no 1.9 ORNL MODEL Q-2792 CONTROLLED- case were reduction waves noted. To get valid polaro- POTENTIAL DC POLAROGRAPH AND ORNL grams, additional supporting electrolyte was necessary MODEL Q-2942 POLAROGRAPHIC for all fractions tested. From the survey of fractions DROP-TIME CONTROLLER collected from the chromatographic column, it seems - that the polarographic technique can not be used as a H. C. Jones R. W. Stelzner direct monitor of the column effluent. This is especially W. L. Belew T. R. Mueller true for the elution conditions (i.e., buffer system) now M. T. Kelley in use. The concentration of buffer salts up to fraction D. J. Fisher 40 are not adequate as a supporting electrolyte. Also, sparging and the addition of a maximum suppressor Companion papers that describe the ORNL model seems to be necessary. The two-cell modes, although Q-2792 controlled-potential dc polarograph’ and workable under laboratory conditions, do not seem Q-2942 polarographic drop-time controller7 are being feasible for direct monitoring with the restrictive prepared for publication. Packages of diagrams and conditions imposed by the current elution system. specifications for fabrication of the polarograph and Indications are, however, that more pertinent monitor- drop-time controller were sent to 18 requesters in the ing information could be obtained under column U.S.A. and to 10 requesters abroad. At the Lucas elution conditions that would provide a more basic Heights Research Establishment of the Australian effluent and one that has a higher concentration of Atomic Energy Commission, both the Q-2792 and the buffer salts. Q-2942 units were duplicated and are working well. Useful information, especially for compounds in the pyridine group, can be secured by the polarographic 1.10 DESIGN OF TIME-AVERAGINGAND TIME- technique in laboratory analyses. Both qualitative iden- DERIVATIVE CIRCUITS FOR DC POLAROGRAPHS tification and quantitative estimation of some of the R. W. Stelzner compounds eluted from the column should be possible. It is evident, however, that fractions from the column A paper is being prepared for publication that may have to be concentrated or possibly extracted from describes the mathematical design techniques which the elution medium and then examined under more have produced the analog circuitry in several of the favorable polarographic conditions. More clearly de- ORNL dc polarographs. fined reduction waves appear in solutions more basic than 0.1 M sodium acetate. 1.1 1 INSTRUMENT FOR END-POINT DETECTION If further polarographic work is contemplated on IN BIPOTENTIOMETRIC TITRATIONS these compounds, it is recommended that a complete L. Belew T. M. Florence’ polarographic survey of each compound be made in W. well-buffered solutions over the pH range 1 to 12. Only Bipotentiometric titrations are done by observing the in this way can all the pertinent identifying character- potential developed across two indicator electrodes in a istics of these compounds be determined, that is, the stirred solution during the passage of a small highly influence of pH on half-wave potentials, the separation of true and catalytic hydrogen-reduction waves, the explanation of the reduction mechanisms, and the 7W.L. Belew, D. J. Fisher, H. C. Jones, M. T. Kelley, T. R. determination of the number of electrons involved in Mueller, and R. W. Stelzner, “Controlled Potential DC Polar- the reductions. Additional polarographic work on these ograph-Voltammeter (ORNL Model Q-2792),” And. Chern. compounds is strongly recommended. Div. Ann. Prop. Rept. Oct. 31, 1967, ORNL-4196, p. 3. 6

stabilized current. The apparatus usually consists of a compare well with those attained by other methods. In pair of platinum electrodes, a large ballast resistor, and the Karl Fischer titration, a 200-mV change in potential a source potential - all in The developed at the end point is observed for additions of as little as potential is measured with a high-impedance voltmeter 0.003 ml of Karl Fischer reagent (e15 pg of H20). such as a pH meter. When high sensitivity and accuracy Thiosulfate solutions as dilute as 1 X lo-’ N were are desired, a stable current is required. In the simple titrated with 0.005 N iodate solutions with an end apparatus just described, the current is made increas- point error <0.01 ml. Further work will be done with ingly independent of cell characteristics by increasing the instrument to evaluate its sensitivity and stability. the source potential and the size of the ballast resistor. However, at very high resistances, response times 1.12 CONTROLLED-POTENTIAL CONTROLLED- increase and leakage currents may become a factor. An CURRENT CYCLIC VOLTAMMETER instrument was fabricated that includes an operational T. R. Mueller H. C. Jones amplifier which produces a highly stable cell current that is essentially independent of the electrode or cell A paper that describes the cyclic voltammeter dis- characteristics. cussed previously2 -’ was submitted for publication. The instrument incorporates a Philbrick P65QU oper- Engineering drawings and a parts list are available.2 ational amplifier to force a constant current through the cell. This amplifier has unusually low power 1.13 DERIVATIVE CIRCUITS FOR USE WITH THE requirements; therefore, mercury batteries can be used CONTROLLED-POTENTIAL CONTROLLED-CURRENT efficiently as a power supply, thus making the appara- CYCLIC VOLTAMMETER tus inexpensive and portable. The cell is placed in the circuit by connecting one electrode to the amplifier T. R. Mueller D. L. Manning24 output and the other electrode to the inverting input of Preliminary studies are in progress to determine the the amplifier. A small bias current (-0.5 pA) is applied requirements for the design of a differentiator (or at the inverting input by a 30-Ma resistor connected to purchase of a commercially available unit) to be used the +15-V power supply. Thus, a constant current of with the cyclic voltammeter (Sect. 1.12). The use of -0.5 pA is forced through the cell. The potential derivative techniques is expected to increase the accu- developed across the electrodes is measured at the racy2’ and sensitivity26 of the determination of output of the amplifier with a microammeter and low-level constituents such as corrosion products in suitable scaling resistors to provide a full-scale output of MSRE fuels. 0.5 and 1.0 V. This simple circuit has several advantages over the use of large resistors in series with a potential source. The 20T. R. Mueller and H. C. Jones, “Controlled-Potentia1 and cell current is independent of the conditions of the cell Controlled-Current Cyclic Voltammeter,’’ Anal. Chem Diu. and electrodes. The potential developed across the cell Ann. Progr. Rept. Oct. 31, 1966, ORNL-4039, p. 1. can be measured with a low-impedance voltmeter, thus IT. R. Mueller, “Controlled-Potential and Controlled- eliminating the need for a high-impedance instrument, Current Cyclic Voltammeter,’’ presented at the Analytical such as a pH meter, to measure the cell potential. The Chemistry Instrument Demonstration Conference, An Industrial cell current is easily adjusted to provide the optimum Cooperation Conference, Oak Ridge National Laboratory, Oak current density at the electrodes without affecting Ridge, Tenn., Oct. 16-17, 1967. current stability (witlun the error limits of the ampli- 22T. R. Mueller and H. C. Jones, “Controlled-Potential Controlled-Current Cyclic Voltammeter,’’ Anal. Chem Diu. fier). Ann. Progr. Rept. Oct. 31, 1967, ORNL4196, p. 1. The instrument has been used for Karl Fischer deter- 3Anonymous, “Controlled-Potential and Controlled-Current minations of water in organic solvents and for iodine- Cyclic Voltammeter,” revised CAPE-1653, Engineering Mate- thiosulfate titrations. The sensitivity and accuracy rials List, TID-4100. 24Reactor Projects Group. 25T. R. Mueller, “On the Separation of Half-Wave Potentials ti J. T. Stock, Amperometric Titrations, Interscience, New Required for Resolution of Simple, Reversible, Overlapping York (1965) pp. 59-60; vol. XX of Chemical Analysis, ed. by Waves in Stationary Electrode Voltammetry,” Chem Instr. 1, P. J. Elving and I. M. Kolthoff. 113 (1968). 9E. Bishop, “Differential Electrolytic Potentiometry. Part 11. 26S. P. Perone and T. R. Mueller, “Application of Derivative Precision and Accuracy of Applications to Redox Titrimetry,” Techniques to Stationary Electrode Polarography,” Anal. AnaIyst 83, 212 (1958). Chem 37, 2 (1965). 7

1.14 ON THE SEPARATION OF HALF-WAVE consists of a Philbrick P25AU operational amplifier and POTENTIALS REQUIRED FOR RESOLUTION OF PR30C power supply provides full-scale output at the SIMPLE, REVERSIBLE, OVERLAPPING WAVES recorder for a photomultiplier-tube current of lo-’ IN STATIONARY-ELECTRODE VOLTAMMETRY amp. The following commercial components are incor- porated into the model IX system: EM1 type 9558QA T. R. Mueller photomultiplier tube, Fluke model 4 12B high-voltage The requirements for the simultaneous determination power supply, Jarrell-Ash Ebert model 82-000 scanning of two or more species by linear-potential-sweep volt- spectrometer, and a Heath EUW20A recorder. A Beck- ammetry at stationary (plane or sphere) or quasi- man oxy-hydrogen burner and burner housing are stationary (expanding sphere) electrodes are discussed mounted on an optical bench from the Jarrell-Ash in a note published in Chemical Instrumentation. Company. One quartz lens is used to focus the image of the flame on the entrance slit of the monochromator. 1.15 MODIFICATION OF DUAL SET-POINT This instrument, now being used by the Radioiso- VOLTAGE COMPARATOR (ORNL MODEL 4-2950) topes-Radiochemistry Laboratory, was constructed to be a reliable replacement for an ORNL model Q-1457 H. C. Jones T. R. Mueller flame spectrophotometer that had been in use for The operational-amplifier feedback network in the several years. ORNL model Q-2950 comparator2 was modified to eliminate occasional double-triggering that occurred 1.18 USE OF STATISTICAL TECHNIQUES when it was used with input signals that change very IN FLAME PHOTOMETRY slowly. The comparator now operates reliably and has D. J. Fisher R. W. Stelzner H. C. Jones been tested with inputs in the range 100 mV/min to 20,000 V/sec. The sensitivity limit of any measurement is set by the statistical characteristics of the noises that inevitably 1.16 INTEGRATOR MODULE accompany the analytical signal. Statistical techniques, including correlation in the frequency and in the time H. C. Jones T. R. Mueller domains, can optimize and enchance the signal-to-noise An inexpensive operational-amplifier current integra- ratio and thus increase sensitivity. A paper has been tor‘ was designed for H. H. Ross.” The integrator has prepared which describes a demonstration that ensem- three ranges. The ratio of the time constants of the ble averaging increases the sensitivity of flame photom- three ranges can be trimmed to within *0.01%. Total etr~.~O charges of 0.1 to 100 microcoulombs can be measured 1.19 INSTRUMENTATION FOR ANALYTICAL with a maximum error for worst-case design of f 1% in 4 min. The minimum input resistance is 3 Ma. Full-scale BIOCHEMISTRY output voltage is +lo V. The integrator is very compact; W. L. Maddox it is packaged in a 5 X 6 X 831, in. box. The prototype tRNA analyzer described pre-

1.17 MODEL IX FLAME SPECTROPHOTOMETER viously3 93 has been replaced by an improved model. The new apparatus functions in the same way in the H. C. Jones R. W. Stelzner overall analytical scheme, that is, it removes fractions The flame spectrophotometer designated model IX, from the analytical product stream by depositing them formerly model VI-C,29 was assembled and has been installed in Building 3026. A dc-amplifier system that 30D. J. Fisher, R. W. Stelzner, and H. C. Jones, “The Use of Ensemble Averaging to Increase the Sensitivity of Measurements with Flame Photometers,” submitted to Chemical Instrurnenta- 27T. R. Mueller, “Dual Set-Point Voltage Comparator (ORNL tion. Model Q-2950),” Anal. Chem Diu. Ann. Progr. Rept. Oct. 31, 31W. L. Maddox, “Instrumentation for Analytical Bie 1967, ORNL-4196, p. 2. chemistry,” Anal. Chem Div. Ann. Progr. Rept. Oct. 31, 1967, 28Nuclear and Radiochemistry Group. ORNL-4196, p. 9. 29R. W. Stelzner, M. T. Kelley, and H. C. Jones, “Model VI 32W. L. Maddox and M. T. Kelley, “An Automatic Sampler Flame Spectrophotometers,” Anal. Chem Diu. Ann. Progr. for Obtaining Discrete Samples from the Output of a Con- Rept. Oct. 31, 1967, ORNL-4196, p. 10. tinuous Flow Analyzer,” Chem Instr. 1, 105 (1968). 8 on filter-paper disks. The precision and speed of substantial further enhancement of S/N. This work was analysis with the new unit are similar to those of the done with a specific wired-program computer - a prototype. The new unit differs in that the sampling signal-averaging computer. A program has been initiated operation is electrically synchronized with the Tech- to explore analytical applications of a general-purpose nicon input sampler rather than with a photometric digital instrument computer system. controller at the proportioning-pump output. Provision is made to automatically start the output sampler 14 to 1.21.a Capabilities 20 samples after the input sampler has been started; also, once started, the output sampler will continue Their Instrument Computer system has been pur- chased from Fabri-Tek Instruments, Inc., Madison, automatically until 40 samples - the number contained Wisconsin 5371 1. The system is a wired-program digital in the input-sampler tray - have been taken. The output sampler then stops automatically. Adjustments computer that combines the flexibility of a general- are provided to phase the sample taken with the desired purpose computer and the Of ‘peration Of a portion of the output stream. laboratory instrument. The program can be varied by selection of switch positions and plug-in modules. 1.20 COMPUTER-ASSISTEDANALYTICAL The system consists of: CHEMISTRY Component Description R. W. Stelzner FT-1064 main-frame 4096-word magnetic-core unit memory (18 bits/word, A 4K-word-memory, integrated-circuit, digital com- 1-psec access time) puter - the Digital Equipment Corporation’s model Plug-in module, SD-1 digitizer, (12 or 8)- PDP 8/I - has been ordered for a study of possible digitizer bit, resolution, applications of data acquisition and on-line real-time linearity of f0.05% computing in the Division. It has been demonstrated3 of full scale SD-2 digitizer, (10 or 6)- that where analytical methods are computer-assisted bit resolution, they have greater accuracy and precision as well as linearity of f0.1% greater throughput. After an initial period of familiari- of full scale zation, the PDP 8/I computer will be evaluated for a (Each digitizer can function as an experiment molten-salt voltammetric problem. To facilitate the interface) development of suitable interfacing, a system of logic Plug-in module, sweep SW-1 control, dwell-time modules has been purchased also. control ranges 200 psec to 0.8 sec SW-2 control, dwell-time 1.21 ANALYTICAL APPLICATIONS OF A DIGITAL range 50 psec to 200 msec INSTRUMENT COMPUTER SYSTEM (Each unit programs the digitizer, arithmetic, and D. J. Fisher D. R. Martin34 memory operations) W.L. Maddox R. W. Stelzner Oscilloscope Tektronix type 503 (Monitors on expanded It has been shown that flame-photometric sensitivity calibrated scales can be improved by statistical means. Sensitivity is the analog-tedigital increased with a flame spectrophotometer that pro- converter output, memory duces an optimized signal-to-noise ratio (S/N) and that contents, and trials of data-processing options) is followed by ensemble a~eraging,~33 which gives FT-201 decimal Prints on paper 120 printer characters per second 33J. W. Frazer, “Digital Control Computers in Analytical (as many as 4096 data Chemistry,” Anal. Chem 40(8), 26A (1968). prints in <4 min) 340RAU Student Trainee from Sacramento State College, X-Y recorder Linear or logarithmic Sacramento, Calif. (Other read-out devices, readout 3SD. J. Fisher, R. W. Stelzner, and H. C. Jones, “Enhance- including tape can be obtained.) ment of Flame-Photometric Sensitivity by Increasing Signal-te Noise Ratio (S/W with a Signal-Averaging Computer,” Anal. Gem Div. Ann &on. Rep. Oct. 31, 1967, ORNL-4196, pp. For digital acquisition of each set of data, quarter, 11-12. half or full memory can be used. Data processing can be 9

Q performed with the main-frame unit prior to readout. laboratory test instrument. The output of a portion of Processing options include: additive or subtractive an instrument, such as a voltage follower, precision acquisition of successive sets of data, data normaliza- peak follower, sample-and-hold circuit, or amplifier, can tion, scaling, complementation, single or multiple inte- be quantitatively compared with its input. Also, the gration, and data transfer. The original or processed output of a derivative-computing circuit can be inte- - data stored in a quarter or half of the memory can be grated and compared with the input. The system can be added to or subtracted from information stored in any used to obtain the logarithrmc or the n’th integral other quarter or half of the memory. Important transform of a measurement. The response (single or separate processing capabilities are the correction of averaged observations) of instrument circuits to stand- data for background and the quantitative comparison of ard test signals can be obtained and then read out to data with other data. The FT-201 prints out the original slower recording devices. During the design of an and/or processed data and also the number of measure- instrument, the system can be used to establish which ment sweeps made on the data. measurement conditions are optimum. The perform- The system is applicable to the measurement of any ance of D.M.E.’s has been examined and tested with variable that can be locked to a sync pulse and observed this system. as a function of a second variable. Just as software can be written to specifically program a general-purpose 1.21.d Use for Digital Polarography digital computer, so can plug-in modules be purchased or designed and wired for specific hardware program- Work was begun to determine what use digital data ming of this digital computer system. There are two acquisition has in polarography. The enhancement of chief modes of digital data acquisition: one sweep per sensitivity that can be obtained by ensemble averaging measurement (for fast, precise measurement followed is being investigated. Later, possibly in conjunction by processing and/or readout to slower analog or digital with the average-mercury-flow-rate control device (Sect. recording devices) and ensemble averaging (with or 1.4) the precision obtainable with an optimum time without further data processing). Each measurement scale will be determined. Also, it is planned to compare sweep can start either with the sync pulse that is locked current-time D.M.E. wave forms. Special attention will to the experimental variable or after a selected delay be given to the study of the early portion of drop time. As many as 8192 sweeps can be programmed by growth in relation to the various accepted equations. the Autostop switch. Also, the system can be used to Results obtained by the mathematical resolution of control or automate experiments and, at the same time, overlapping digital polarographic waves will be com- to acquire and process data from the experiments. Its pared with first-derivative dc polarograms obtained output can be interfaced to a general-purpose digital earlier.3 Other polarographic work planned with this computer. system includes the reevaluation of third-derivative dc polarography and the design of D.M.E.’s having im- proved S/N ratios. 1.21.b Planned Use with Special Interfaces It is expedient for the experimenter to acquire the 1.22 INFORMATION PACKAGES SUBMITTED ability to design, build,. and modify interfaces between TO THE DIVISION experimental equipment and a digital-computer system. OF TECHNICAL INFORMATION EXTENSION Digital Equipment Corporation’s Logic Kits and asso- W. L. Belew W. L. Maddox ciated digital and analog equipment have been pur- H. C. Jones T. R. Mueller chased so that interfaces for specific purposes can be built on a standard breadboard panel. It is planned to Each CAPE package consists of a description of an use the Fabri-Tek Instrument Computer system with instrument or apparatus, a list of references, copies of interfaces built for special applications. the drawings, a parts list, and specifications for fabrica- tion. The material is duplicated and offered for sale by the Clearinghouse for Federal Scientific and Technical 1.21.c Use as a Laboratory Test Instrument The Fabri-Tek Instrument Computer system will be 36D. J. Fisher, W. L. Belew, and M. T. Kelley, “Recent used to collect data essential to the rational design and Developments in D. C. Polarography,” pp. 89-134 in vol. 1 of testing of components, circuits, and systems for other Polarogaphy 1964, ed. by G. J. Has, Macmillan, London, instruments. In this application, it serves as an excellent 1966. 10

Information (CFSTI), Springfield, Virginia 221 5 1. The sional groups who are using the instruments and Engineering Materials List (TID4100 and its supple- apparatus developed in our group, we have consulted ments) is a catalog of the items available from CFSTI. concerning their operation and maintenance. We have submitted to DTIE the following revised or Within the ORNL organization, we have assisted the new packages: Chemistry Division in the design of a voltage-follower amplifier system for an electrochemical measurement; CAPE No. Title we have cooperated with the Instrumentation and Controls Division in the check-out of a cyclic voltam- 368 “Automatic Potentiometric Titrator” (revised) meter (ORNL model Q-2942); and we have consulted 1196 “High-Sensitivity Coulometric Titrator with Reactor Chemistry Division personnel concerning /Q-2564/” (revised) the application of the cyclic voltammeter and have 1220 “Servo-Controlled Pipetters” (revised) assisted in the design of a high-input impedance 1651 “Polarographic Drop Time Controller amplifier system. For the Process Instruments Mainte- /Q-29421” nance Group (4500s Instrument Shop) of the Instru- 1652 “Controlled-Potential D.C. Polarograph- mentation and Controls Division, a series of six lectures Voltammeter /Q-2792/” on operational amplifiers in analytical instrumentation 1653 “Controlled-Potential and Controlled- were delivered - their purpose was to help the Current Cyclic Voltammeter” instrument technicians who must service the equip- ment. Outside the laboratory, we have had fabricated for 1.23 COOPERATIVE PROJECTS the USAEC New Brunswick Laboratory some critical parts for an ORNL model Q-1348B servo-pipetter; for D. J. Fisher the University of Tennessee Hospital in Knoxville, we and checked out an ORNL model Q-l988A polarograph Group prior to its loan. We have sent on loan to .the Through consultation and design efforts, the Analyt- Department of Chemistry at Purdue University the ical Instrumentation Group has cooperated with groups prototype model of the conductivity titrator, and we in the Analytical Chemistry Division and in other have arranged the loan of a servo-pipetter display to the ORNL divisions and with people outside the Labora- United Technical Corporation, West Concord, Mass. tory. Within our own division, we have consulted with With personnel of Lawrence Radiation Laboratory, the Reactor Projects Group on molten-salt instrumenta- Livermore, Calif., we have cocperated in the interpreta- tion, the Methodology Group on a constant-current tion of voltammetric data from multicomponent sys- coulometric problem, the Methods Development and tems through use of our computer program CHICAL Evaluation Laboratory on the measurement of uranium and CURRENTS. To Professor A. F. Krivis of the by high-precision single-cell dc polarography, and the University of Akron, diagrams and information about General Analyses Laboratory on a special valve problem the ORNL model Q-2792 polarograph were furnished in vacuumfusion technology. With the various divi- for use in a book he is writing. p. Analytical Methodology

W. D. Shults

2.1 GAS CHROMATOGRAPHY added, namely: high-purity helium, argon, and ; two unassigned high-purity gas systems; and clean air. A 2.1 .a Instrumentation high-vacuum system and outlets for natural gas, oxygen, M. R. Guerin high-pressure process air, and house vacuum complete the services on the center benches. Similar services are The gas chromatographic capabilities of the Division installed at wall stations to provide for the operation of have been extended with the acquisition of a bio- console instruments. medical gas chromatographic system. It consists of two All gas cylinders and vacuum pumps are located in the column-bath units and an electronics unit and has the attic above the laboratory, but the associated regulators usual thermal-conductivity and dual hydrogen-flame- and electrical switches are located within the labora- ionization detectors for routine use. The system fea- tory. The purity of the service gases to the chromat- tures gas- and solid-sampling capability, an all-glass ographic system is ensured by constructing connecting analytical flow train, capillary-column capability, multi- lines of stainless steel and by Heliarc welding all linear temperature programming, high-temperature elec- connections that are not easily accessible. tron-capture detection, flame-photometric detection One 8-ft laboratory hood was removed from each side (phosphorus- and sulfur-specific), and simultaneous of the laboratory. On one side, the hood was replaced operation of all detectors. The system allows the with storage cabinets; on the other, the Varian- separation, partial characterization, and quantitation of Aerograph preparative gas chromatograph and vented microgram and submicrogram amounts of most non- cabinets for the storage of organic solvents will be macromolecular organic compounds. installed. The modifications were designed with the assistance 2.1 .b A Remodeled Laboratory of G. R. McNutt,' and the changes are being made for Gas Chromatography under the supervision of F. L. Hannon.2 A. D. Horton' C. M. Boyd' A. S. Meyer' 2.1 .c Device for Sampling Gases Contained One of the "wet-chemistry'' laboratories in Building in Sealed Metal Tubes 4500s is being remodeled specifically for gas chroma- A. D. Horton' C. M. Boyd' M. R. Guerin tography to effect more efficient use of the floor and storage areas and to eliminate potential safety hazards The gases contained in Geiger-Mueller (G-M) tubes now associated with instrument maintenance. were collected for mass spectrometric analysis by use of A major modification is the separation of the two a puncturing device (Fig. 2.1). The G-M tube is inserted center benches to form a 2-ft-wide unobstructed aisle in a 'h-in.-OD copper tube that is connected at one end between their backs. This aisle gives safe access for to a vacuum pump and at the other end to a sample maintenance of the bench-top chromatographs. All bulb. The entire system is evacuated, and the device is services for these instruments are conducted through a isolated from the vacuum system by closing a valve (not 6-in.-wide chase that runs full length at the rear of each shown). The G-M tube is punctured by a sharp blow on bench. There are no backsplashes on the benches, and the welding rod with a hammer. A portion of the very short connections can be used to provide the gas sample enters the sample bulb, which is sealed off with and electrical services to each instrument. a torch. A bulb with a vacuum stopcock may also be All unneeded services have been eliminated, for used. This device has been used to puncture copper example, water with accompanying drains and about tubing having 0.035-in.-thick walls. It can be used for half the air, natural-gas, and house-vacuum outlets. The any soft-metal tubing or for thin-walled tubing of any services required to operate the chromatographs were metal if the outside diameter of the tube does not exceed 'I16 in.

'Reactor Projects Group. 2General Engineering Division. 12

A

ORNL-DWG. 68-12473 ORNL-DWG. 68-1247d

STAINLESS STEEL WELDING ROO v I I I I I I TEFLON SLEEVE (l/8- in.-diom I Column, 10-ft by 1/4-in. stainless stee Tributyl Packing, 0.15wt % Carbowax 20-M Phosphate SAMPLE BULB on 60- to $0-mesh siliconized (94.31mole%: glass beads OR OTHER SEALED METAL TUBE Helium flow, 60cc/min Attenuation, 200

'-3/4-in. SWAGELOK FITTING

Fig. 2.1. Device for Sampling Gases in Sealed Metal Tubes.

Methyldibutyl 2.1 .d Biomedical Applications Phosphate 1 (0.95 mole %) M. R. Guerin

The biomedical gas chromatographic system has been Hold 235°C Prog. 9'/min --_-I 110°C 4 used to study free fatty acids, phenylthiohydantoin Dimethylbutyl Decompositior Product! derivatives of amino acids, and trimethylsilylphenyl- Phosphate Trimethyl thiohydantoin derivatives of amino acids. Valeric, iso- (0.93 mole % 1 phosphate (0.95 mole%) valeric, myristic, palmitic, and stearic acids were used to establish conditions for the separation and detection of submicrogram quantities of C4 to C3 saturated fatty acids. The conjoint use of silylation and flame- 1 I photometric detection appears to be highly promising 1680 (440 1200 960 720 480 240 0 for the analysis of phenylthiohydantoin derivatives of RETENTION VOLUME, cc amino acids. Fig. 2.2. Gas Chromatogram of a Mixture of Trimethyl 2.1 .e Determination of the Methyl Esters Phosphate, Dimethylbutyl Phosphate, Methyldibutyl Phos- of Butyl Phosphoric Acids phate, and Tributyl Phosphate. A. D. Horton' The Chemical Technology Division is studying exten- eluted at temperatures as much as 125°C below their sively the degradation of tributyl phosphate (TBP) by boiling points. The column is operated routinely with nitric acid. The decomposition products are phosphoric, ester concentrations as low as 0.01 mole % when the butyl phosphoric, and dibutyl phosphoric acids. That flame-ionization detector is used. If the sample size is Division prepared methyl esters of these acids by increased, concentrations as low as 0.001 mole 76 can be diazotization; trimethyl phosphate (TMP), dimethyl- measured. butyl phosphate (MMBP), and methyldibutyl phosphate (MBBP) are obtained. 2.1.f Determination of These esters are separated from each other and from Perfluoromethylcyclohexane in Methane TBP on a 10-ft by 'h-in. stainless steel column that is A. D. Horton' packed with 60- to 80-mesh siliconized glass beads coated with 0.15 wt % Carbowax 20-M. The column is The Radiation Physics Section of the Health Physics operated at a helium flow rate of 60 cc/min and is Division is studying electron attachment to fluorinated programmed to 235OC at 9"/min after an isothermal hydrocarbons and the life of the attachment to these period of 8 min at llO°C. Figure 2.2 shows the compounds. A sample of methane that contained chromatogram. perfluoromethylcyclohexane (C7 F14) in very low con- The outstanding feature of the low-loaded glass-bead centration was submitted for the determination of column is that the easily decomposed compounds are C7F14. This compound is an analog of methylcyclo- 13 hexane and has about the same boiling point. However, valve, which is normally closed, was replaced with a columns that are suitable for separating methylcyclc- Viton diaphragm. Benzene and its derivatives cause hexane from methane did not adequately resolve neoprene to swell. An inordinately high pressure is methane and C7F14;the C7F14 peak appeared on the required to inject a sample onto the column through a tail of the relatively large methane peak. swollen neoprene diaphragm. The Viton diaphragm Perfluoromethylcyclohexane was separated satisfac- allows a uniform low pressure to be used and thus torily from methane on an 8-ft by ‘h-in. stainless steel provides more reproducible injection volumes. The life column packed with 30- to 60-mesh Burrell medium- of the Viton diaphragm has not been determined; the activity silica gel coated with 3 wt % squalene. The first one has given satisfactory service since its instal- helium flow was 60 cc/min; the column was operated lation in February 1968. isothermally at 62°C for 4 min and then was tempera- ture programmed at 6”/min to 125°C. The flame- 2.1 .h Derivative Gas Chromatography ionization detector was used. The retention volume of R. W. Morrod J. A. Dean6 methane was 66 cc and that of C7F1 4 was 630 cc. The M. R. Guerin W. D. Shults concentration of C7F14 in the only methane sample submitted was 0.17 pl (liquid) per liter of methane. We have initiated a program of study in derivative gas chromatography. Ths program will comprise the doc- 2.1 .g Preparative Gas Chromatography toral research for R. W. Morrow. The objective of the A. D. Horton’ J. D. Lodmel13 first phase of this project has been to develop a detector that is specific for organosilicon compounds. A flame- The organic compounds listed in Table 2.1 were photometric detector for silica has been built and purified by preparative gas chr~matography.~ tested. Its performance is adequate, but work is continuing with the intent of improving sensitivity. This Table 2.1. Organic Compounds Purified phase of the work has been conducted largely at the by Preparative Gas Chromatography University of Tennessee, but the subsequent work will be done within the Division laboratories. Purity Achieved Compound (mole %)

Acetonitrile >99.99 2.2 THIN-LAYER CHROMATOGRAPHY Aniline >99.99 1-Bromobenzene 99.96 2.2.a Instrumentation 1-Bromobutane 99.98 1,6-DimethyInaphthalene 99.96 Helen P. Raaen Dimethylbutyl phosphate (crude) 96.76 2-Ethylnaphthalene >99.99 The Chromoscan was received from Joyce, Loebl & Methyl formate >99.99 Co., Ltd. on April 1. The instrument is a recording and Propionitrile >99.99 integrating densitometer, absorptiometer, and color- n-Propylbenzene >99.99 imeter for reflectance and transmittance operations in 2,2,6,6-Tetramethylheptane-3,5-dione 29.99 the visible and ultraviolet on various types of samples. 1,1,l-Trichloroethane 99.98 1,1,2-Trichloroethane >99.99 The thin-layer scanner attachment arrived on July 26, N-Valeric acid 99.95 and the power supply for its ultraviolet light source was pXylene >99.99 received on August 16. However, the ultraviolet light source has not yet come. The scanner attachment will Only one significant change has been made in the be suitable for reflectance and transmittance measure- Varian-Aerograph preparative gas chromatograph. The ments in the visible and ultraviolet on thin-layer neoprene diaphragm in the pressure-time sampling chromatograms of various types.

30RNL Student Trainee under the ORNL Undergraduate Program; present address, University of Tennessee, Knoxville. ’Student Guest from the Department of Chemistry, Univer- 4A. D. Horton, “Prepaative Gas Chromatography,” Anal. sity of Tennessee, Knoxville. Chem Div. Ann. Progr. Rept. Oct. 31, 1967, ORNL-4196, p. 6Consultant; Professor of Chemistry, University of Tennessee, 33. Knoxville. 14

2.2.b Polytetrafluoroethylene (Teflon) as an Adsorbent sional TLC on polyethyleneimine-cellulose is described Helen P. Raaen in a published article.’ The summary from the article follows: We have done experimental work to develop poly- “A method is given for resolving a complex mixture of nucleic tetrafluoroethylene (Teflon) layers for thin-layer chro- acid bases, nucleosides, and nucleotides on polyethyleneimine- matography (TLC). A description of the details of the cellulose MN-300 chromatofilms. The nucleotides are prevented from migrating when the individual nucleic acid bases and work will be reserved for publication as a journal nucleosides are separated from each other. Also, in the course article; a summary follows: of the development that resolves the nucleotides, the nucleic Teflon slurries of numerous compositions were eval- acid bases and nucleosides disappear. Thus, the procedure uated for forming the Teflon layer. Layers were made simplifies the isolation and detection of individual components whose properties are entirely satisfactory for TLC. of a complex mixture of nucleic acid derivatives. The method was applied satisfactorily to the analysis of alkali hydrolysates These properties include rate of drying, uniformity, of the transfer ribonucleic acids of E. coli B and of yeast.” adherence to a support (glass, and Mylar or vinyl film), wettability by test-solution aliquot and developer, rate 2.2.d Amanita Toxins of development, and resolution of the components of a test mixture. It was demonstrated that the layers are Helen P. Raaen suitable for both partition and reversed-phase partition Thin-layer chromatography was used to follow the chromatography, depending on how the liquid compo- progress of the production of amanita toxins by nents of the chromatographic system are distributed fermentation growth of the mycelium of the mushroom between the stationary phase on the thin layer and the Galerina marginata. During this work, some improve- mobile developer. A thin layer of Teflon was found to ment in an existing TLC separation was achieved. In a be a suitable solid support for the selected liquid note accepted for publication,’ this improvement is anion-exchanger acid di<2-ethylhexyl)-orthophosphoric described and is illustrated with color photographs of (HDEHP); two multicomponent mixtures of cations pertinent chromatograms. were separated on such a layer by both partition and reversed-phase partition TLC. This finding invites a 2.2.e Steroids detailed study of the use in TLC of liquid ion exchangers, of which many exist. In addition, it Linda J. Cristl Helen P. Raaen indicates the potential usefulness of thin layers of Teflon (a chemically inert material) for studying the In the Body Fluids Analyses Program, it is of interest mechanism of extractions with liquid ion exchangers by to detect, identify, and quantitatively measure steroids means of TLC without the need to consider the in urine. Work was begun to apply TLC in the solution reactivity of the solvent system with the solid support, of these problems. Because of the large number (>600) a factor that must be considered when most other TLC and the complexity of the steroids that may be present adsorbents are used. Also, Teflon was shown to be in urine, their separation by TLC can be exceedingly compatible in thin layers with alumina and with silica difficult. The experimentation to date has consisted in gel in any ratio. The possibility therefore exists of showing that a selected TLC system is satisfactory for including Teflon as a component of mixed-adsorbent the immediate work, obtaining reference data for pure and gradient layers for TLC and thus, on a single layer, of simultaneously effecting adsorption and partition 70RAU Student Trainee from Nazareth College, Nazareth, TLC in any controlled ratio to each other. Ky.; summer, 1967. 8H. P. Raaen and F. E. Kraus, “Thin-Layer Chromatography Extensive and exciting experimental work with Tef- of Constituents of Transfer Ribonucleic Acid (tRNA),” Anal. lon as a TLC adsorbent is possible. First consideration is Chem Div. Ann. Prop. Rept. Oct. 31, 1967, ORNL-4196, pp. being given to corrosive (e.g., HF-containing) systems 34-35. for which existing adsorbents (e.g., silica, alumina, the ’H. P. Raaen and F. E. Kraus, “Resolution of Complex celluloses, and the like) are not suitable and to the Mixtures of Nucleic Acid Bases, Nucleosides, and Nucleotides by Two-Dimensional Thin-Layer Chromatography on Polyeth- difficultly separable transuranium elements. yleneimine-Cellulose,” J. Chromatog. 35, 5 3 1 ( 196 8). ‘OH. P. Raaen, “Thin-Layer Chromatography of Amanita 2.2.c Constituents of Transfer Toxins,” Anal. Chem Div. Ann. Progr. Rept. Oct. 31, 1967, Ribonucleic Acid (tRNA) ORNL-4196, p. 35. ’ H. P. Raaen, “Improved Thin-Layer Chromatographic Helen P. Raaen Frances E. Kraus7 Separation of Amanita Toxins on Silica Gel G Chromatoplates,” accepted for publication in the Journal of Chromatography. Our work’ to resolve complex mixtures of nucleic 120RAU Student Trainee from Arkansas State University, acid bases, nucleosides, and nucleotides by two-dimen- Jonesboro. 15

steroids and steroid conjugates, determining the limit of Fluorescence is among the most sensitive means for detection for four steroids and a steroid conjugate, detection. analyzing samples provided from the column chroma- Of particular interest is the observation that andros- tography of urines by the Body Fluids Analyses Group, t er on e, 1 1 -dehydrocorticosterone, 50-pregnane- and evaluating the TLC system as a means to follow the 3a,2k-diol diacetate, A4 -androsterone-3,11,17-trione, course of acid and enzymatic hydrolysis of steroid 170-estradio1, estriol, and estrone, on layers sprayed conjugates. Also, information was accumulated on with 1:1 H2SO4 (conc.) and heated at 78"C, phospho- possible methods for the quantitative measurements of resce under liquid nitrogen after excitation with ultra- submicrogram amounts of steroids isolated by TLC. violet light. This characteristic of these steroids has not, The TLC system found to give satisfactory resolution to our knowledge, been reported before. A note on this of 20 steroids of primary interest includes: adsorbent, observation has been prepared for publication in the Merck Silica Gel G in 250-p-thick layers on Mylar film Journal of Chromatography. Low-temperature phos- (or glass); developer, chloroform-methanol (97:3 v/v); phorescence of steroids appears to have received only and development, 15 cm in a developer-saturated limited study; it should have most interesting possibil- atmosphere. Gelman ITLC-SA medium is an equally ities. satisfactory adsorbent. The developer dichlorometh- The TLC system was applied to the analysis of 16 ane-acetone (70:30 v/v) also causes the steroids to samples of interest in the column chromatography of migrate on Merck Silica Gel G, but in a slightly urine. The results did not show conclusively the different order. Therefore, it may be a suitable devel- presence of any one of the standard steroids studied. oper for use in a two-dimensional system for resolving However, several components were isolated that are complex mixtures of steroids. now undergoing identification tests. The chromatograms are analyzed both before and The TLC system was shown to be a means to follow after they are sprayed with 1 : 1 H2S04 (conc.) and the hydrolysis of steroid conjugates. Samples of three heated to 78OC. The analysis consists in observing the pregnanediols and a pregnanediol glucuronide were chromatograms for color, absorbance, fluorescence, and chromatographed simultaneously with the HC1-hydroly- phosphorescence both in air and immersed in liquid sis product of the pregnanediol glucuronide. Each of nitrogen under visible, 366-nm ultraviolet, and 254-nm the pregnanediols and the glucuronide were isolated ultraviolet light. satisfactorily. In the product, pregnanediols were iden- For the 21 pure reference steroids and the 10 tified, but numerous other products of the hydrolysis conjugated steroids that constitute the collection of the were also indicated to be present. Body Fluids Analyses Group, reference TLC informa- tion has been accumulated and cataloged. It can be 2.2.f Mass Spectrometry of Substances retrieved when sought according to either the name of Isolated by Thin-Layer Chromatography the compound or the conditions under which the W. T. Rainey' Helen P. Raaen presence of a resolved component on the thin-layer Linda J. Crist' chromatogram is evident. For some selected compounds, their limits of detec- Mass spectrometry can be used to identify and tion on the thin layer by observation of fluorescence at possibly to quantitatively measure some substances room temperature were determined by sequential dilu- isolated by TLC. The method is of increasing interest tion. The developed chromatogram was sprayed with for organic substances. The mass spectra of several TLC 1:1 H2S04 (conc.) and then heated at 78OC on a hot adsor bents (polytetrafluoroethylene, polyethylene- plate to form products that are colored in visible light imine-cellulose, Sephadex G-75, polyolefin, Merck Sil- and that fluoresce under 254-nm ultraviolet light. The ica Gel G, Corning porous glass 7935, Gelman ITLC-SA compounds and their detection limits were: medium, alupina) were recorded on the low-resolution mass spectrometer to determine the extent of their Micrograms Compound background interferences in the mass spectrometry of Detectable Not Detectable substances held on them. The inorganic adsorbents behave better than the organic. The silicic adsorbents 17-Hydroxydeoxycorticosterone 0.1 0.01 1 1-Dehydrocorticosterone 1 0.1 cause little or no interference; the interference from Cortisone 1 0.1 5a -Pregnane-3p,20p-diol 1 0.1 Pregnanediol glucuronide 1 0.1 ' Mass and Emission Spectrometry Group. 16

polytetrafluoroethylene is acceptable, and that from total-condensate sample was extracted with cyclo- polyolefin is not. hexane. The cyclohexane extract was then extracted with nitromethane to give a solution enriched in 2.2.g Infrared Spectrometry of Substances polynuclear aromatic hydrocarbons. Part of the cyclo- Isolated by Thin-Layer Chromatography hexane-extracted methanolic solution was filtered M. M. Murray’ Helen P. Raaen through a lipophilic resin to give a fraction enriched in Linda J. Crist’ polar components. An aliquot of the ethereal total- condensate sample was fractionated into basic, pheno- Infrared spectrometry is an established way to iden- lic, acid, and neutral portions by solvent extraction. tify organic substances. A technique in which Wick- The neutral portion was subjected to further fractiona- Sticks (wedge-shaped pieces of compressed KBr) are tion on silica gel. Portions of each solution were taken used effects the removal of a TLC-isolated substance at appropriate stages in the fractionation and concen- from the adsorbent onto KBr for subsequent infrared tration procedures to yield samples that corresponded spectrometry. This technique is being evaluated with to various levels of condensate handling. Gas chroma- corticosterone isolated by TLC on a Merck Silica Gel G tographic profiles are to be obtained for each fraction layer and on Gelman ITLC-SA medium. to find whether significant chemical fractionation oc- curs in the condensate-collection apparatus and to 2.3 CHARACTERIZATION OF TOBACCO measure the influence of the various fractionation and SMOKE AND SMOKE CONDENSATES concentration procedures on the contents of the frac- tions. A program was begun to develop analytical method- ology to definitively characterize tobacco smoke. The 2.3.b Thin-Layer Chromatography approach proposed is to selectively remove compounds Helen P. Raaen of given classes, such as polynuclear aromatic hydro- , inorganic gases, and alkaloids, from tobacco Information has been collected on the application of smoke or smoke condensate and to determine the TLC to the isolation and identification of the compo- compounds simultaneously as classes and individual nents of tobacco-smoke condensates. Bibliographic in- components. Gas chromatography, with its high resolv- formation was received from the National Clearing- ing power, high sensitivity, and general applicability, house for Smoking and Health, the National Library of appears to be the analytical method of choice. Medicine, and 21 organizations listed in the publication “1967 Directory of On-Going Research in Smoking and 2.3.a Exploratory Studies Health” as doing analyses on tobacco smoke. Also, M. R. Guerin references were extracted from the “1 967 Bibliography on Smoking and Health.” The most abundant informa- Thus far, experimental work has been done to gain a tion came from Dr. R. L. Stedman of the Tobacco further appreciation of analytical difficulties peculiar to Laboratories, Agricultural Research Service, U.S. De- cigarette smoke and smoke-condensate matrices. The partment of Agriculture, and from Dr. E. Sawicki of the condensate from 500 cigarettes in each of the five trap Particulate Chemistry Section of the National Center sections of a smoking apparatus (Sect. 10.11.b) was for Air Pollution Control. The material was searched divided into ether-soluble and ether-insoluble portions; carefully and indexed. Unfortunately, it includes very the ether-insoluble condensate was dissolved in metha- few references on the application of TLC. nol. The ethereal solutions and methanolic solutions This scarcity prompted a search of the entire Journal were concentrated. Samples of the ether-soluble frac- of Chromatography. Information was sought in partic- tion and methanol-soluble fraction of the total conden- ular on ways to separate polynuclear aromatic hydro- sate were obtained by combining aliquots of the carbons, alkaloids, and phenols, which are three types ethereal concentrates and methanolic concentrates, of compounds of importance in the analysis of tobacco respectively. smoke condensates. Also, attention was given to articles The total condensate samples were subjected to that describe unusual techniques of analysis or that chemical fractionation. An aliquot of the methanolic suggest unique overall approaches to the general prob- lem of the analysis of tobacco-smoke condensates. The search was very fruitful, and the references of interest 141nfraed and N.M.R. Group. have been indexed. 17

A memorandum was prepared on the possible role of The results of the study of the analyzer and TLC in the analysis of tobacco-smoke condensates. The relative ease with which methane, hydrogen sulfide, and memorandum calls attention to newer techniques that phosphine can be stripped from water suggest that it warrant consideration during our work in this area. may be possible to develop an aqueous-injection gas chromatographic system for estimating the total car- 2.4 ANALYSIS OF WATER SYSTEMS bon, sulfur, and phosphorus (and perhaps total nitro- gen) contents of aqueous solutions. 2.4.a Aqueous-Injection Gas Chromatography M. R. Guerin W. J. Ross W. D. Shults 2.4.b Eutrophic Water Systems

Samples for gas chromatography are often in organic W. J. Ross solvents. When the compounds to be determined are In association with members of the Health Physics present in aqueous solution, they are normally recov- Division, 15 sites have been monitored for phosphorus ered in an organic solvent and subsequently determined and nitrogen to study the origin and movement of algal in that solvent. Applications of the direct gas chroma- nutrients in local watersheds.’ A Technicon Auto- tographic analysis of aqueous solutions (aqueous-injec- Analyzer was acquired to measure very low concentra- tion gas chromatography) are becoming increasingly tions (5 to 100 ppb) of phosphorus as P043- and important with the intensified interest in determining nitrogen as NO2- or NO3- by the molybdenum blue and the organic components of biological fluids and natural diazo (sulfanilamide-naphthylethylenediamine) colori- water systems. Accordingly, we have begun to study metric methods, respectively. Measurements were made means for, and applications of, aqueous-injection gas on untreated samples, as well as on those that had been chromatography. treated to convert organic phosphates and inorganic An aqueous-injection gas chromatographic tech- metaphosphates to orthophosphate ions. nique” for the quantitative determination of the total A highly polluted water system was analyzed by carbon content of aqueous solutions has been studied. activation analysis. The objectives were to establish the Microliter volumes of aqueous samples are injected onto effect of Mo, Cu, P, Mn, and Zn on the growth of a bed of hot (850°C) copper oxide over which a carrier chlorella algae and to determine the effectiveness of gas (nitrogen or helium) passes continuously. The hydroponic beds of rye and fescue to remove these carbon in the sample is converted by the hot copper elements from flowing streams of water. This work was oxide to . The carbon dioxide is mixed done in cooperation with members of the U.S. Depart- with hydrogen, and the mixture is swept by the carrier ment of Agriculture, who initiated the program. gas through a heated (300°C) packing to produce methane. The methane is swept onto a gas chromato- 2.4.c Deaeration Systems graphic column and is measured in the column effluent with a flame-ionization detector. Whereas for methane W. J. Ross the limit of detection (<1 ppm total carbon) and the A reliable chemical method was needed to evaluate shape of the detector response are good, it has been instruments designed to measure very low concentra- difficult to obtain reproducible quantitative results for tions (1 to 100 ppb) of dissolved O2 in saline water and total carbon. The problem may be associated with the also as a “standard” method to be used in acceptance necessity to inject the sample by syringe through a tests of future desalination plants. The Winkler method silicone rubber septum. was adapted for the determination of dissolved 02 in The possibility of applying aqueous-injection gas water from any source. The work has consisted prin- chromatography to the determination of dissolved gases cipally in identifying and eliminating all interferences has also been examined. Conditions have been estab- and has included the modification of colorimetric lished that allow methane, air, carbon dioxide, hydro- methods for Fe2+, Fe3+, Cu+, and Cu2+ for use in the gen sulfide, and phosphine to reach an analytical determination by field laboratories of ppb amounts of column while water is being retarded long enough to be these ions. Methods are also being developed to remove vented from the system. these interferences from discrete samples or flowing

”F. R. Cropper, D. M. Heinekey, and A. Westwell, “The Determination of Total Organic Matter (Carbon Content) in l6 W. J. Ross, “Analysis of Water Systems,” Anal. Chem Div. Aqueous Media,” Analyst 92, 436 (1967). Ann. Prop. Rept. Oct. 31, 1967, ORNL-4196, p. 87. streams of deaerated water without altering the concen- determine manganese and copper in samples of human tration of dissolved 0’. Chelating reagents and columns tissue by activation analysis. Complete removal of of chelating ion-exchange resins have been applied milligram amounts of sodium from 1 to 12Nsolutions successfully to fresh-water systems but have not been of HCl, HN03, and HzS04 can be achieved by tested with saline water. Continued investigation of the adsorption of sodium on small (0.5-g) columns of HzC03 HC03 =+ COz equilibria and additional Sb’ 05.The ions Mn” and Cu” are not retained when modification of a revised ASTM method’ ’ for deter- the acidity is 6 to 12 N; therefore, the gamma mining COz in saline water have been required to radioactivity from 56Mn and 64Cu can be measured in ensure reliable analyses of brackish water that contains the eluate without interference from ’ Na. Related very high concentrations (200 to 500 ppm) of dissolved experiments have shown that K+ and Cs+ are com- CO’ . pletely adsorbed on a column of Sbz05 when the acid These analytical methods were used in a large number concentration of the elutriant is 1 M. However, the of performance tests to evaluate the deaeration system degree of adsorption diminishes with increasing acidity. of the Desalination Facility at Roswell, New Mexico, Therefore, both K+ and Cs+ are completely eluted in which is operated by the Office of Saline Water, and the >9 M HN03 and can be separated quantitatively from experimental deaeration equipment designed and in- Na+ . stalled at ORNL. The ions Mn2+ and Cu2+ can also be separated from Na+ by adsorption on a column of Chelex-100 cation- 2.4.d Fluorometric Determination of Phosphate chelating resin. When the pH of the sample solution is in the range 2 to 4, Mn’+ and Cu’+ are completely J. C. Guyon’ W. D. Shults adsorbed and Na+ is rejected. Sodium ions are not The work on the fluorometric determination of adsorbed at pH’s <4; Mn’+ and Cu” are retained phosphate was reported previously.” An article on it completely only at pH’s >2. Therefore, the buffer 0.1 has now been submitted for publication in the Journal M acetic acid-0.1 M sodium acetate is used to ensure of the American Water Works Association. quantitative separation.

2.5 SEPARATION AND CONCENTRATION 2.5.b Evaluation of a Lipophilic Adsorption Resin STUDIES for Desalting and Removing Organic Compounds from Water 2.5.a Column Chromatography with M. R. Guerin

W. J. Ross Amerlite XAD-2, a highly lipophilic polystyrene adsorption resin manufactured by the Rohm and Haas A study of the efficacy of Sbz O5 for isolating sodium Company, has been examined as a medium for re- ions’ - especially dangerous or interfering amounts of moving low-molecular-weight water-soluble organic ’‘Na+ - has been continued as part of a program to compounds from large volumes of acetate buffer. The ability of the resin to adsorb organic compounds from dilute aqueous solutions suggests that the resin may also 17. ’Total Carbon Dioxide and Calculation of the Carbonate be useful for removing organic compounds from natural and Bicarbonate Ions in Industrial Water,” ASTM Method No. waters for further analysis. D 513-57, pp. 29-34 of I964 BookofASTMStandards, pt. 23, American Society for Testing and Materials, Philadelphia, Pa., Batch-extraction procedures were used to assess the 1964. potential utility of XAD-2. When 7-ml volumes of wet ’80RAU Research Participant; Associate Professor of Chem- XAD-2 were in contact for 24 hr with 40 ml each of -5 istry, University of Missouri, Columbia. X M aqueous solutions of sec-butylamine, piperi- 19J. C. Guyon and W. D. Shults, “Fluorometric Determina- dine, 3-indoleacetic acid, and hippuric acid, the resin tion of Phosphate,” Anal. Chem Div. Ann. Prop. Rept. Oct. 31, 1967, ORNL-4196, p. 40. adsorbed 65, 54, 72, and 94%, respectively, of the test ’OJ. C. Guyon and W. D. Shults, “Rapid Survey Methods for compound. For 0.05, 0.1, 1, and 2 M solutions of the Fluorometric Determination of Phosphate,” submitted for acetate buffer (pH 4.4) under the same conditions, the publication in the Journal of the American Water Works resin extracted 16, 15, 17, and 17% of the acetate, Association. 21 W. J. Ross, “Separation of Sodium with Antimony Pent- respectively. When the resin and test solution were oxide,” Anal. Chem Div. Ann Progr. Rept. Oct. 31, 1967, transferred to a glass-wool-plugged separatory funnel ORNL-4196, p. 88. and washed with distilled water, 99% of the acetate a‘ 19

buffer was removed from the sample, whereas of that Caution must be exercised in applying the technique originally present -40% each of the sec-butylamine, to solutions that contain large amounts of inorganic piperidine, and hippuric acid and -90% of the indolea- salts. Salt deposited in the chamber alters the evapora- cetic acid were left on the resin. The facts that acetate tion rate and thus necessitates frequent adjustments in is removed from the resin and the test compounds were the flow rate of the air and/or delivery rate of the not completely stripped from the resin strongly suggest solution. that large amounts of inorganic salts could be very Because the chamber remains cool throughout the easily removed from very small amounts of organic concentration procedure and because concentration is compounds by use of XAD-2. achieved at atmospheric pressure, the dangers of chem- It is concluded that this liquid-solid extraction pro- ically altering or volatilizing the solute are minimized. cedure affords a simple and effective approach to An inert gas may be substituted for air in those cases greatly reducing the contamination of small amounts of where contact with atmospheric constituents must be organic compounds by common salts. The conclusion is avoided. based on considerations of the influence of pH, sample volume, resin volume, and sample concentration on 2.5.d Concentrating Hydrochloric Acid resin uptake and on a comparison of liquid-liquid W. J. Ross extraction by use of ethyl acetate, ether, n-butanol, and benzene with liquid-solid extraction using XAD-2. In the course of a series of experiments in which C1 Although fitration through XAD-2 is definitely a way was adsorbed on oxide electrodes, a technique was to remove organic compounds from natural waters, its developed whereby C1, as H3 C1 in aqueous solution, relative merit for this purpose compared with filtration can be concentrated by removal of water without loss through carbon remains to be determined. of the valuable C1 radionuclide. This procedure Amberlite XAD-2 is being evaluated further as a consists simply in controlled dehydration, in a closed scavenger of organic compounds from natural waters system, of the H3 Cl solution through preferential and as a medium for adsorption chromatography. removal of water vapor from the solution by a pool of concentrated H2S04. Solutions that were 0.1 to 0.5 N 2.5.c Device for the Unattended Concentration in H36C1 were concentrated to 1 to 5 N in four days of Solutions with a loss from the H36Cl of <1% of the 36Cl originally present. M. R. Guerin

A means has been devised for the unattended 100- to 2.6 AIR QUALITY SURVEY 1000-fold concentration of the solutes in organic M. R. Guerin W. D. Shults solutions. By an infusion pump that drives a 10-ml syringe, the solution is fed continuously into a small At the request of the Melton Hill Regional Industrial evaporation chamber while the solvent is removed byan Development Association, the levels of potential air aspirating stream of air through the chamber. Loss of pollutants were sumeyed at Eagle Bend Industrial Park, solute to the walls of the chamber is minimized by Clinton, Tennessee. Airborne sulfur, , maintaining a very small liquid volume within the halogens, and reducible metals were collected by chamber (50 to 100 pl). An evaluation of the tech- drawing air through gas-dispersion bottles filled with nique by use of n-eicosane as a solute in diethyl ether solutions of sodium hydroxide. Particulate matter was indicates that solute recovery can be quantitative. collected by drawing air through 0.45-p Millipore Chamber geometry influences the rate of evaporation fdters. Air-sampling rates were controlled with needle of the solvent. A higher rate is achieved by venting the valves on the vacuum pumps used to sample the air and aspirating air parallel to and directly above rather than were measured with calibrated flowmeters. Collection perpendicular to the sample zone of the chamber. The times varied from 24 hr to 5 days over a period of rate of evaporation is highly dependent on the flow rate about 30 days. Airborne low-molecular-weight organic of the aspirating air. A study of 22 solvents shdwed that compounds were collected by opening a previously the time necessary to reduce 10 d.of solvent to 10 to evacuated 40-liter bomb sampler at the sampling site. 100 pl ranges from 30 to 90 min for solvents such as Several capabilities within the Division - including diethyl ether and n-hexane to 15 to 20 hr for solvents service analysis, mass spectroscopy, and gas chroma- such as dimethyl sulfoxide and n-butanol. tography - were applied to the determinations of the 20

compounds of interest. Table 2.2 summarizes the Work is under way to redetermine the half-lives of results. 241 Am and 243Am by measurement of absolute alpha radioactivities and coulometric determinations of Table 2.2. Levels of Air Contaminants at the Eagle masses. Bend Industrial Park, Clinton, Tennessee

Contaminant Level (pg/m3) 2.7.b Titrimetric Determination of Americium

sulfur 30 J. R. Stokely W. D. Shults Nitrogen dioxide <17 Fluoride Undetectable We investigated the possibility of determining amer- Halide other than F- Undetectable icium by redox titrimetry. Direct titration of Am(VI) Metals (Cd) 3 with Fez+ proved unsatisfactory, because the reaction is Total particulates 10 sluggish in the end-point region. Attempts to accelerate Total hydrocarbons (0.10 ppm v/v) the reaction by heating and by titrating in strong-acid medium were unsuccessful. Similar behavior was ob- served with several types of indicator-electrode systems. It is concluded that the quality of the air at the Eagle An indirect procedure that involves adding excess Fez+ Bend Industrial Park is far superior to that of typical to reduce the Am(VI) and then titrating the excess Fez+ urban areas and, in many respects, is superior to that of with a standard solution of dichromate was also most nonurban areas for which comparable information studied. This approach gave analytical results that were is available. The detection of measurable amounts of erratic and inaccurate by several percent. We believe what seems to be cadmium is consistent with reports that the limitation common to both these procedures is that a nearby industry makes heavy use of cadmium that it is impossible to prepare Am(V1) quantitatively alloys. The operation of the Bull Run Steam Plant does and free of excess oxidant. Accordingly, the procedures not appear to contribute significantly to ground-level do not appear to have promise, and this work has been sulfur. terminated.

2.7 RESEARCH AND SUPPORT ACTIVITIES 2.7.c Micro Titration of Plutonium IN THE TRANSURANIUM RESEARCH LABORATORY J. R. Stokely W. D. Shults Work is under way to extend the titrimetric method 2.7.a Controlled-Potential Coulometric of Drummond and Grantz4 to the determination of Determination of Americium semimicro and micro amounts of plutonium. The J. R. Stokely W. D. Shults method consists in chemical oxidation of Pu(II1) to h(VI), reduction of Pu(VI) to Pu(1V) with an excess of Further work on the controlled-potential coulometric Fez+, and titration of the excess Fez+ with a standard determination of americium’ comprised a study of solution of dichromate. The purpose of this work is to precision, accuracy, and several possible interferences. offer an accurate and precise alternate to the presently The work is now complete. An article on it has been used coulometric method in which iron and large submitted for publication? the abstract follows: quantities of sulfate interfere. The method appears to “Controlled-potential coulometry has been studied as a means for the precise and accurate determination of americium. have potential usefulness. Americium is chemically oxidized to the hexavalent state, and then coulometrically reduced from the hexa- to the pentavalent 2.7.d Voltammetric Studies of Plutonium, Neptunium, state at a platinum electrode controlled at 1.05 V vs. S.C.E. The and Americium results of repetitive analysis of standard solutions prepared from high-purity americium dioxide agree within a few tenths percent J. C. Guyon’ W. D. Shults with standard values for 0.4 to 1.0 mg of americium.” We have initiated a program to study the voltam- metric behavior of the lighter transuranium elements. z2J. R. Stokely and W. D. Shults, “Contxolled-Potential Coulometric Determination of Americium,” Anal. Chem Div. Ann Progr. Rept. Oct. 31, 1967, ORNL4196, p. 89. 23J. R. Stokely and W. D. Shults, “Controlled-Potential 24J. L. Drummond and R. A. Grant, “Potentiometric Coulometric Determination of Americium,” submitted for Determination of Plutonium by Argentic Oxidation, Ferrous publication in Analytica Chimica Acta. Reduction and Dichromate Titration,” Talantu 13,477 (1966). 21

We tested a rotating (600 ipm) pyrolytic-graphite 2.7.f Separation of Californium electrode and a rotating platinum-disk electrode for this J. R. Stokely work and found the platinum electrode to be more satisfactory. The voltammetric behavior of plutonium To assist members of the Chemistry Division in in mineral-acid media has been examined in some detail, determining the (n,~)cross section of ”’ Cf, californi- and that of neptunium has been examined in an um was separated chemically from fission products and exploratory manner. Our results indicate that voltam- actinides. The separation consisted in a metry may be useful for rapid ionic determinations of fluoride precipitation, separation of the actinides from these ions in various oxidation states and for studying the lanthanides on a cation-exchange column with 12.5 the effects of various reagents and complexing agents M HC1-20% ethyl alcohol as the eluting solvent, and on these ions. These studies have revealed possible ways finally the separation of californium from einsteinium to eliminate the interferences of iron and Pu(VI) in the on a small “but” column. The purified californium controlled-potential coulometric procedure for deter- fraction contained <1% of the original einsteinium and mining plutonium; these means are being pursued. We -80% of the californium. Other details of this work are have also examined briefly the voltammetric behavior presented in a recent report.2s of Am(II1) but did not obtain promising results with that ion. 2.7.g Reparation and Analysis of the 0-Diketones of the Lanthanides and Actinides 2.7.e Modification and Installation of Perkin-Elmer Model 240 Elemental Analyzer in a Glove Box J. R. Stokely J. R. Stokely Assistance was given in the preparation of the ameri- cium and the chelates of hexafluoroacetylace- Several modifications were made on the Perkin-Elmer tone and 2,2,6,6-tetramethyl-3,5-heptanedione.The model 240 Elemental Analyzer to permit analysis of compounds were analyzed for americium, carbon, samples inside a glove box. The major alterations were hydrogen, nitrogen, and water. One of the compounds to place the combustion furnace inside the box and to is reasonably volatile and probably can be used for va- extend the gas lines outside to the Analyzer. The por-pressure and gas-chromatographic studies. Details of purpose of the alterations was to prevent contamination I this work are being published.2 of the electronics and gas-analysis sections of the Analyzer. Since water is a product of combustion, it 2.7.h Purification of Am and Am was necessary to heat the exit gas line to 300 to 350°C to prevent condensation and adsorption of water vapor J. R. Stokely in the line. Standard acetanilide from the National Bureau of Several batches of 241Am and 243Am were purified Standards was used to check the calibration of the to meet a need for high-purity americium in the analyti- Analyzer. The calibration factors, which relate recorder cal chemistry and other research programs at the Trans- readout from thermal-conductivity detectors to weight uranium Research Laboratory. Because of the radiation of carbon, hydrogen, and nitrogen in the sample, were hazard, the sizes of the batches had to be limited to 300 the same as values obtained before modifications were to 500 mg. The purification method consisted in three made. The consistency indicates that the instrument is precipitations of americium(V) carbonate, operating properly. In addition, several pure organic elution of Am(II1) from an anion-exchange column compounds were analyzed, and the results obtained were within the Perkin-Elmer specifications. Several 25C. E. Bemis, J. Halperin, and J. R. Stokely, “The Neutron highly radioactive samples have been analyzed, and no Capture Thermal Cross Section and Resonance Integral of radioactivity has been transferred out of the glove box 252Cf,”Chem Div. Ann hog. Rept. May 20, 1968, ORNL- through the gas lines. Liquids that have low vapor 4306, p. 22. pressures can be analyzed for carbon and hydrogen with 26M.D. Danford, J. H. Burns, 0. L. Keller, Jr., J. R. Stokely, and W. H. Baldwin, “Prepuation and Volatilities of Some Rare- the instrument by altering the automatic combustion Earth and Americium Chelates,” submitted for publication in cycle. the Jouml of Physical Chemistry. 22

with 8 N HCI, several precipitations of americium 2.8.b Rapid Polarography of Uranium in 1 M hydroxide with ammonium gas, and a final precipita- Hydrofluoric Acid with a Vertical-Orifice Telfon tion of americium from weak acid solution. The Dropping-Mercury Electrode oxalate was converted to the dioxide by ignition in air at 900°C. Emission spectrographic and radiochemical An article3 that describes the rapid polarography of analyses revealed no detectable impurities except that uranium in 1 M HF with a vertical-orifice Teflon D.M.E. one batch contained -1 wt % . is to be submitted for publication; the abstract follows: “The polarographic characteristics of uranium, as 2.7.i Spectrophotometric Determination of Plutonium U02(N03)2, in 1M HF were studied with a rapid, vertical- J. C. Guyon’ J. R. Stokely W. D. Shults orifice dropping-mercury electrode (dme) of polytetrafluoro- ethylene (Teflon, du Pont trade-name). The study shows that The work on the spectrophotometric determinations this type of dme is satisfactory for rapid polarography in glass-corroding media. Within the span of potential from +0.6 to of plutonium was reported previously27 and now has -1.5 V vs. a saturated calomel electrode (sce), two polare been published.’ graphic waves were observed. At E112 -0.55 V vs. sce a reproducible wave of excellent form exists, for which the 2.8 POLAROGRAPHIC STUDIES WITH THE relations of C to id and of C to (dadt),,, are linear and the TEFLON DROPPINGMERCURY ELECTRODE plots pass through the origins. The wave is therefore both qualitatively and quantitatively useful. Dissymmetry in the (D.M.E.) first-derivative peak of the wave suggests that the reduction is Helen P. Raaen irreversible. A second polarographic wave appears at E112 2 +0.3 V vs. sce. This wave is reproducible and its height is a 2.8.a Evaluation of Vertical-Orifice Rapid Teflon function of uranium concentration, although the C us. id relation appears not to be linear. The fist-derivative peak of the D.M.E.’s for Obtaining Fundamental wave is unsymmetrical. The wave is easily distinguished from Polarographic Data the mercury-dissolution wave. It is relatively large - possibly \ catalytic - and may be the basis for a highly sensitive An article2 on the evaluation of vertical-orifice Tef- polarographic method for uranium.” lon D.M.E.’s was accepted by Chemical Instrumentation for publication. The summary from the article follows: “A vertical-orifice dropping-mercury electrode (dme) of poly- 2.8.c Polarography of (Sulfite) tetrafluoroethylene (Teflon, Du Pont trademark) was fabri- in Aqueous Hydrofluoric Acid cated and evaluated for rapid polarography in glass-corroding media. The oritice is in a vertical face of the Teflon segment of The following is the summary from an article ac- the dme capillary, which is positioned vertically. Capillaries of cepted for p~blication:~’ orifice diameter from about 70 to 120 p were made. The gee “A well-formed polarographic wave exists for sulfur dioxide metric and performance characteristics of the dme were studied. (sulfite) in aqueous hydrofluoric acid at a half-wave potential Polarograms of T1+, Cda, and UOza were recorded; the sup (El/2) of about -0.4 V us. a saturated calomel electrode porting media were aqueous hydrofluoric acid or acid chle (S.C.E.). The characteristics of the wave are similar to those of ride solutions. The polarographic characteristics of the ref- the wave for sulfite in aqueous solutions of hydrochloric acid erence reaction T1+ * T1° in 0.1 M KCl-lmM HCI were deter- and of nitric acid. The relation of sulfite concentration (0to mined to permit comparison of this dme with horizontal-orifice diffusion current (id) is linear, and the wave is reproducible. glass and Teflon dme’s, for which similar data have been pub- Polarography in aqueous hydrofluoric acid media is indicated tg lished. Results obtained with polyacrylamide present as a maxi- be a suitable method for the detection and direct quantitative mum suppressor agree with the known polarographic charac- measurement of sulfur dioxide. Possible significant applications teristics of the T1+ =.+ T1° reaction. They thus show that the of the method are to determine contaminative sulfur dioxide in vertical-orifice dme of Teflon is satisfactory for the rapid polar- hydrogen fluoride gas, in reagent-grade hydrofluoric acid and ography of glass-corroding media.” fluorosulfuric acid, and in the atmosphere.”

27J. C. Guyon and W. D. Shults, “Spectrophotometric Deter- mination of Plutonium,” Anal. Chem. Diu. Ann. Progr. Rept. Oct. 31, 1967, ORNL-4196, p. 40. 28J. C. Guyon, J. R. Stokely, and W. D. Shults, Spectrophe 30H. P. Raaen, “Rapid Polarography of Uranium in 1M tometric Determination of Total Plutonium: Observations on Hydrofluoric Acid with a Verticalarifice Polytetrafluore the Reactions Between Arsenazo and Pu(III), Pu(Iv, and ethylene Dropping-Mercury Electrode,” to be submitted for Pu(VI), ORNL-TM-2108 (Jan. 2, 1968). publication. H. P. Raaen, “Vertical-Orifice Dropping-Mercury Electrode 31Helen P. Raaen, “Polarography of Sulfur Dioxide (Sulfite) of Polytetrafluoroethylene for Rapid Polarography in GlassCor- in Aqueous Hydrofluoric Acid,” accepted for publication in roding Media,” to be published in Chemical Instrumentation. Amlytica Chimica Acta. 23

2.9 EVALUATION OF THE PERFORMANCE standard material for sulfide; hence, one is forced to OF ION-SELECTIVE ELECTRODES “standardize” the standard solution. This standardiza- tion is a nuisance, especially because standard sulfide W. D. Shults solutions are not stable. Second, concentrations of We have evaluated the performance of the Orion sulfide in solution depend very much on pH - H*S, sulfide electrode. This is a solid-membrane type of HS-, and S2- are in mutual equilibria - and therefore electrode that is advertised to measure sulfide concen- the acidity must be either controlled very carefully or trations as small as lo-’ ’ M with no interferences. The measured. At some pHs, the sulfide concentration may electrode does respond to very low concentrations of be extremely low and yet total sulfur concentration sulfide, but the total surfur concentration must not be may be very large. This condition may to gross M for satisfactory response. For several reasons, inaccuracies in detehining total sulfur, since one use of this electrode is much more complicated than is measures sulfide and computes total sulfur from the the use of the other ion-selective electrodes we have sulfide measurement for the pH that prevails. Third, ~tudied.~First, there is no completely satisfactory calibration curves may exhibit marked curvature. Be- cause of these difficulties, we prefer to use the sulfide electrode as an indicator electrode for titrations rather than as a device for direct potentiometry. In the D. Shults, A. F. Roemer, Jr., and S. S. Potterton, 32W. indicator function, the electrode performs beautifully. “Evaluation of the Performance of Ion-Selective Electrodes,” Anal. Chem Div. Ann Progr. Rept. Oct. 31, 1967, ORNL- When sulfide is titrated with , potential changes 4196, p. 36. that are -1 V in magnitude occur near the end point.

/’

A. S. MeyeI J. M. Dale

3.1 MOLTEN-SALT REACTOR EXPERIMENT result for an earlier sample (FP-7-9) whose analysis was deliberately delayed to accentuate the effects of radia- 3.1.a Determination of Oxide in MSRE Salts tion and with the average of the results of all fuel by Hydrofluonnation analyses since the reactor achieved power operation. R. F. Apple A. S. Meyer J. M. Dale Whereas the absolute standard deviation (+8 ppm) of the sampling-analysis procedure is satisfactory, the Because the earlier analyses by the hydrofluorination method’ had established that a low and essentially Table 3.1. Oxide Concentrations of MSRE Fuel Salt constant concentration of oxide could be maintained in the MSRE fuel, the determination of oxide in reactor Oxide Sample Date Special Concentration salt samples was assigned a lower priority during this Designation Treatment (PP4 period of operation. Table 3.1 compares the results of the two oxide analyses performed on the fuel with the FP-14-39 12-2-68 None 46 FP-14-53 2-7-68 Heated carrier 58 FP-7-9 7-4-66 Stored 24 hr at 50 cell temperature ‘R. F. Apple and J. M. Dale, “Determination of Oxide in Average of all samples (15) analyzed since 54k8 MSRE Salts,” Anal. Chem Div. Ann Progr. Rept. Oct. 31, reactor start-up 1967, ORNL-4196, p. 15. 24 accuracy of the method for radioactive samples is Table 3.2. Oxide Concentrations of Samples difficult to establish. A possible source of error is the from Test Runs and from 233UFuel Concentrates loss of oxygen because of radiolysis during the -8-hr J Sample Oxide Sample interval between sampling and analysis; it is known that Sampler Weight Concentration Designation fluorine is generated radiolytically during this period. (& (PP4 Sample FP-14-53 was transported in a carrier that maintains the sample at a temperature above 500°F to LiF-UF4 Pellet 3.5" 1000 eliminate the radiolytic generation of fluorine. Because 25A Copper-sleeve 3.5Q 85 of a crowded sampling schedule, it was not possible to 40 Copper-brass 3.5" 105 analyze many samples transported in the heated carrier funnel before the scheduled reactor shutdown. The facts that 43 Inconel 12.lb 107 minimization of the effects of radiation on the sample 44 Inconel 12.16 117 caused no significant change in the results and that the RU 33-14-2 Fuel Inconel 12.lb 62 overall reproducibility is good strongly suggest that the RU 33-2-S-1 Fuel Inconel 12.lb 33 radioactivity of the samples introduces no determinate RU 33-2-S-2 Fuel Inconel 12.lb 37 error in the method. RU 33-34-1 Fuel Inconel 12. lb 31 When the reactor was not in operation, the hydro- RU 33-34-2 Fuel Inconel 12.lb 32 fluorinator was used to analyze a number of radioactive and nonradioactive samples. Solvent salt (LiF-BeF2) samples for the In-Pile Test Loop were analyzed to determine the source of oxide contamination. The taken for analysis. These sections were placed in results are: standard ladles that were prefitted with a welded Oxide Concentration delivery tube which extended to the bottom of the Sample (PPm) ladle. After the usual preliminary hydrofluorination at 300"C, the sample was melted and allowed to flow to 42 the bottom of the ladle for efficient purging. The 375 62 results confirm the effectiveness of the preliminary 60 hydrofluorination step to remove surface contamina- 62 tion that results from atmospheric exposure. Sample 1 was taken from the original salt preparation. The evaluation of the effects of radiation on the Sample 2 was exposed in the molten state for 96 hr to components of the hydrofluorinator is of considerable the atmosphere of a helium-filled dry box. Samples 3 interest, because it is planned to adapt the technique to through 5 were purged, in series, with helium for 48 hr. the in-line analysis of radioactive salt streams. In The method for oxide was also adapted to smaller general, the experience has been satisfactory. In this samples taken to determine the completeness of re- third year of operation, only three repairs of in-cell moval of oxide from fuel concentrates (LiF-' UF4) components were needed. Two of the failures - leaks in by batch hydrofluorination. Table 3.2 gives the results. the remote coupler resulting from the corrosion of The first five analyses were run to establish optimum nickel ball joint by fumes from an adjacent cell and an sampling techniques; the samples came from a test open circuit in the valve-compartment heater system - preparation of concentrate prepared from normal do not appear to be associated with radiation damage. uranium. This development work was performed with The cause of the desensitization of the electrolytic G. I. Cathers.' Initial samples were taken in a special moisture-monitor cell, the third since the apparatus was sampling system designed to withdraw a filtered sample installed, is subject to question. The first and last in a small copper ladle. To ensure that HF-H2 mixture (present) of these cells, which were used primarily for bubbled through the molten sample, it was necessary to the analysis of samples of relatively low radioactivity, either transfer the sample to a standard ladle or couple a survived at least 20 analyses and eight-month service copper sleeve to the ladle. Larger and more representa- life. Conversely, the other cells, which were used for tive samples were provided by drawing the molten salt samples taken during extended power operation, failed into a '4 -in.-OD Inconel tube. The melt was cooled, and after four to ten analyses and two- to four-month usage. 1-in. sections were cut from the salt-filled tube and All failures have been of the same general type. Plastic components exhibited some evidence of noncritical 'Chemical Technology Division. radiation damage, and the P205 electrolyte was re- 25

@ moved from the electrodes. In an attempt to reproduce ORNL-DWG. 68-2772fi these failures under controlled conditions, a moisture- CALCULATED I monitor cell was operated in the vertical position at EX PER I M ENTA L 65°C. After the repeated analysis of a series of 1.5 relatively large SnOz standards had failed to reduce the \ cell’s efficiency, the cell was removed and subjected to 1.0 -IO7 rads of 6oCo radiation. The irradiated cell I- c continued to function for several months and finally was desensitized after the passage of a total of about 1.5 g of water. This treatment represents an exposure to both radiation and water that is at least an order of I I II magnitude greater than that which produced in-cell 10 20 30 40 failure. Although the in-cell failures may have been due REACTOR INTEGRATED POWER (Mwhr x to the characteristics of the individual moisture moni- tors, it is desirable to investigate other techniques for the measurement of water for application to in-line Fig. 3.1. Concentration of U* in MSRE Fuel Salt. oxide analysis of molten-salt reactor fuels. 3.1 .b Determination of Uranium(II1) rod of beryllium metal was lowered into the fuel in the in Radioactive MSRE Fuel reactor. The beryllium is oxidized by the fuel; this by Hydrogen Reduction reaction results in an increase in the U3+ concentrations. All increases in the calculated U3+ concentrations J. M. Dale R. F. Apple are a result of beryllium additions, whereas the de- A. S. Meyer J. E. Caton creases result from fuel burnup. The analysis of the C. M. Boyd sixth and seventh samples gave HF yields in the The theory of the hydrogen-reduction method for hundreds of micromoles, which do not correlate with U(II1) in radioactive MSRE fuel and the initial evalu- U3+ concentrations. At this point, difficulty was experi- ation of the experimental results were described pre- enced with the sampler station, and the reactor was viou~ly.~It was noted at that time that the results of shut down for about a month and a half for mainte- the U3+ determinations did not reflect the beryllium nance. The first two U3+ results determined after the additions made to the MSRE fuel salt to reduce reactor was brought back to power were close to the fractional percentages of the u4‘ to U3+.However, the calculated values, and the result for the third sample computer program used initially to evaluate the ex- was low. At this point, the reactor was down again for a perimental results did not take into account the change short time. The next U3+ results were increased but in equilibrium concentrations of the corrosion products were still lower than the estimate. One explanation for and uranium that must occur when the fuel is cooled the low U3+ results is that they are caused by the from reactor temperature to the temperature at which radiolytic production of fluorine. This hypothesis was the first hydrogen-reduction step was made. As a result, discussed previ~usly.~To eliminate this source of error, the values previously reported for the U3+ concen- a heated sample carrier was made to transport the fuel trations are those for 500°C, the temperature of the samples from the reactor to the hot-cell facilities (Sect. first reduction step, and not for 663”C, the temperature 3.1.a). Due to sampling problems at the reactor, only of the fuel in the reactor. one U3+ sample so transported was taken before the The computer program has since been modified, and final reactor shutdown. The U3+ result for this sample the experimental results were reevaluated. The new was low compared with the calculated value. On the ratios of U3+ to total U are plotted in Fig. 3.1 and are basis of only one analysis, no conclusions can be drawn compared with the calculated ratios that would be about the importance of using the heated transport expected to exist by virtue of the beryllium additions container. and the fuel burnup. After the first sample was run, a Work was continued to develop a method for the remote measurement of ppm concentrations of HF in 3J. M. Dale, R. F. Apple, and A. S. Meyer, “Determination of helium and in hydrogen gas streams.’ The construction Uranium(II1) in Radioactive MSRE Fuel by a Hydrogen-Reduc- tion Method,” Aml.‘Chern Div. Ann Progr. Rept. Oct. 31, 4Zbid., p. 19. 1967, ORNL-4196, p. 16. ’]bid., p. 20. 26

and calibration of the dual trapping system for the deterioration in the TC-cell response. We have found continuous absorption and desorption of HF on sodium that the sampling of a helium gas stream will serve for fluoride were completed. The trapping system consists this purpose. At a cell current of 270 mA and a i of a dual selector valve, a special monel thermal- flush-gas flow of 100 cc/min, the agreement of the cell conductivity (TC) cell (Cow Mac model 9454) with responses for repetitive samplings of a pure helium gas nickel filaments and two sodium fluoride traps. The stream was better than 0.1%. A 10% change in the valve and TC cell are contained in a Boekel model 1078 flush-gas flow causes a change in the cell response of laboratory oven at 50°C and are connected to the only 1%. sodium fluoride traps, which are mounted on the Provisions are now being made to use the trapping outside walls. This arrangement permits the simultane- system for the analysis of the HF evolved from the ous absorption of HF on one trap at room temperature hydrogen reduction of standard fuel-salt mixtures. This and the desorption of HF from the alternate trap at analysis should provide a check of the validity of the 300°C by means of self-resistance heating. Figure 3.2 hydrogen-reduction method and reveal any of its shows a curve typical of the response of the TC cell to limitations. the desorption of HF from a sodium fluoride trap. The initial smaller peak is due to a small amount of water 3.1 .c Determination of Total Reducing Power impurity and is almost completely resolved from the of Radioactive MSRE Salts HF peak. As shown in Fig. 3.3, integration of the TC-cell response vs the number of micromoles of HF R. F. Apple A. S. Meyer desorbed from the traps is linear over the range of A method is required to determine whether active interest (1 to 50 micromoles of HF). This range colloidal metals, particularly excess zirconium, are corresponds to an HF concentration of about 8 to 400 present in reprocessed MSRE fuel solvent. The estab- ppm at a carrier-gas flow of 100 cc/min and an absorption period of 30 min. When this trapping system for the U3+ determinations ORNL-DWG. 68-101 I is installed in the hot-cell facilities, it will be necessary I , I I I I I I 1' to have some means to check periodically for any

OR N L- DWG. 68-10399A !

$ 0.8 I- 3 0 J J e 0.4 l 0 I-

0 5 10 15 20 0 12 24 36 48 TIME, min HF, micromoles

Fig. 3.2. Thennal-Conductivity-CellResponse Curve for the Fig. 3.3. Thermal-Conductivity-Cell Response vs HF De- Desorption of HF from a Sodium Fluoride Trap. sorbed from Sodium Fluoride. 27

A lished hydrogen-evolution method6 is not applicable to through a combustion tube that contains CuO main- radioactive samples, because a finely powdered sample tained at 700°C. This combustion converts hydro- .I is required. No facilities are available to pulverize carbons in the helium to C02 and H20. The oxidized radioactive samples under a controlled atmosphere. A gas stream is passed through one side of a thermal-con- modification of this technique is being developed in ductivity (TC) cell, through a 3A molecular sieve- which an unpulverized solid sample is dissolved in a A~carite-Mg(C10~)~trap, which removes the C02 and sealed tube in an HCI-HB03 mixture. We have demon- H20, and back through the reference side of the TC strated that 250-mg fragments of fuel, solvent, and fuel cell. The difference between the thermal conductivity concentrate are completely disintegrated by a 24-hr of the gas in the two sides of the cell is a measure of the treatment at 250°C. The sealed tube is protected by an hydrocarbon concentration in the off-gas; the detection overpressure of C02 during the dissolution. In the limit is -10 ppm. A length of brass tubing is installed hot-cell deterinination, the evolved hydrogen will be upstream of the reference side of the TC cell. After the mixed with a standard addition of helium, and the gas stream is switched by means of valves to bypass the H2 /He ratio will be determined mass spectrographically. trap, a step response in the TC signal is obtained. This To simulate the hot-cell operation, samples were added plateau represents the period required to equilibrate the to a tube that was fitted with a breakseal and that oxidized surface of the brass tubing with moisture (Fig. contained a thin-walled ampoule of deaerated acid. The 3.5). By use of standard gas mixtures, it was demon- tube was evacuated and sealed off by using a small strated in a laboratory system that the relative step (-300-W) platinum-wound furnace. The acid-containing heights are proportional (within *lo%) to the ratio of ampoule was then broken by shaking. The dissolution C02 to H20. Therefore, an estimate of the ratio of was completed successfully. Since all these operations carbon to hydrogen in the reactor off-gas can be made appear to be feasible by remote manipulation, an from such measurements. apparatus is being fabricated to perform the disso- The initial tests of the system on MSRE off-gas have lutions and standard additions of helium within the hot shown that the fission-product radioactivity in this cell. stream causes serious interference. This interference results primarily from the radiolysis of traces of 3.1.d Analysis of MSRE Helium for Hydrocarbons absorbed water in the trap rather than from the radiolysis of the reagents themselves and indicates an C. M. Boyd impurity level of the order of 100 ppm. This level A system to measure continuously the total hydro- increased only slightly on oxidation, indicating only carbon concentration in the radioactive off-gas of the about 10 ppm of combustibles. MSRE has been installed in the gas-sampling station. In Tests have been made on the materials contained in this system (Fig. 3.4), the reactor off-gas is passed the trap to determine the effect of radiation. Samples (5-g) were sealed in 20-cc glass vials fded with helium at 50-mm pressure and were subjected to 2 X lo’ rads 6W. J. Ross and J. C. White, “Uranium Triflu0ride.h the Presence of Uranium Tetrafluoride, Hydrogen Evolution Method,” Method No. 9 00720003 (3-28-56), OWL Master ORNL-DWG. 67-366A Analytical Manual, TID-7015,sect. 9. Sample, 200 ppm C4HI0 in Helium Flow Rote, 50cc / min Combustion Tube, CuO at 670°C ORNL-DWG. 67-243A 6 in. x 3/16 in. ID Copper Tubing 2ft x 1/16 in. ID Brass Tubing Fl

*. , ---1 I I I 0 I 234 5 678 TIME, min

Fig. 3.5. Results of the Determination of Hydrocarbons in Fig. 3.4. Flow Diagram of Hydrocarbon Analyzer for MSRE Helium by Measuring the Thermal Conductivity of Their Off-Gas. Combustion Products. 28 of 6oCo radiation. Mass spectrometry showed that reproducibility of voltammograms and chronopotentiograms for hydrogen is the major radiolysis product from Ascarite, the oxidation process is poor, presumably owing to attack of the working electrode by U(VI) produced in the dispropor- whereas oxygen was produced from both wet and dry .I tionation.” samples of Mg(C104)2. Wet molecular sieve gave some H2, N2, CO, and 02.Dry molecular sieve produced 3.2.b Voltammetry of Chromium(I1) in Molten very little contaminant gases on irradiation. The large LiF-BeF2-ZrF4 at 500°C trap that contained the mixture of absorbing materials is being replaced with a small trap that contains only D. L. Manning J. M. Dale molecular sieve. A heater on this trap will keep it free of water and C02 by a bake-out between tests. The The electrochemical reduction of Cr(I1) in molten LiF-BeF2-ZrF4 (65.6-29.4-5.0 mole %) was studied by amount of contaminant gases produced by radiolysis in voltammetry with linearly varying potential. Well- this small dry trap should be greatly decreased. defined voltammograms were obtained with pyrolytic- graphite and glassy-carbon indicator electrodes at a 3.2 ANALYTICAL METHODS FOR THE potential of about -0.9 V vs a Ni/NiF2 reference IN-LINE ANALYSIS OF MOLTEN electrode.” Linear plots of peak current (ip) vs FLUORIDE SALTS concentration were obtained over the concentration 3.2.a Disproportionation of Electrochemically range studied, -0.008 to -0.03 F Cr(I1). Linear plots Generated Utanium(v) in Molten of ip vs (scan rate)’/2 obeyed the Randles-Sevcik LiF-BeF2-ZrF4 at 500°C equation from about 0.02 to 1 V/sec. The diffusion coefficient calculated from the slope of the line is of D. L. Manning Gleb Mamantov’ the order of 1 X cm2/sec at 500°C. In the presence of U(IV), the chromium wave is enhanced, An article was published’ that describes our study of because the Cr(I1) +. Cr(0) reduction occurs at the foot the disproportionation of electrochemically generated of the U(IV) + U(II1) reduction wave. U(V) in molten LiF-BeF2-ZrF4 at 500°C. Certain of In cooperation with T. R. Mueller,’ a first-derivative the results are consistent with theoretical predictions of ’ circuit was assembled and added to the controlled- Fischer and Dr’i~ka.~The summary from the article potential controlled-current cyclic voltammeter. Use of follows: “Electrochemical oxidation of U(IV) has been studieod in the derivative circuit gave much better resolution of the molten LiF-BeFz-ZrF4 (65.6-29.4-5.0 mole %) at 500 by chromium wave in the presence of U(1V); however, the means of voltammetry (scan rate, u, 0.01-100 Vlsec), chrono- first-derivative peak current for the Cr(I1) -+ Cr(0) potentiometry, and chronoamperometry at unsheathed py- reduction was still enhanced by U(IV). rolytic graphite and Pt-lW Rh electrodes. The following From the results obtained thus far, it is believed that results point to the disproportionation of the electre chemically-produced U(V): (a) no voltammetric currents owing the Cr(1k) + Cr(0) reduction wave can be used to the rereduction of the product at u < 1 V/sec, the peak analytically to monitor Cr(I1) in fluoride melts; in the currents (i,) for the oxidation of U(IV) and re-reduction of the presence of U(IV), it could be useful on an empirical product being approximately equal at v $ 1 V/sec; (b) peak basis. currents for the reduction of U(IV) to U(II1) and the oxidation of U(1V) are the same at large scan rates; (c) the observed increase in ip/u1/2 vs. u at u < 1 V/sec; (d) the observed 3.2.c Electromotive Force (EMF) Measurements variation of i0T1l2 with is in agreement with theoretical in Molten Fluorides predictions of Fischer and Dracka’. At Pt-10% Rh electrodes, evidence for the adsorption of U(IV) has been obtained. The H. W. Jenkins’ D. L. Manning Gleb Mamantov7 The program of emf measurements in molten fluo- rides’ was continued; Table 3.3 summarizes the 7Consultant; Associate Professor of Chemistry, Department of Chemistry, University of Tennessee, Knoxville. ‘D. L. Manning and G. Mamantov, “Disproportionation of E1ectrochemically;Generated Uranium(V) in Molten LiF- ‘OH. W. Jenkins, D. L. Manning, and G. Mamantov, “Elec- BeF2-ZrF4 at 500 ,” J. Elechoanal. Chem 18,137 (1968). tromotive Force (EMF) Measurements on the Nickel-Nickel(I1) ’0.Fischer and 0. Dgcka, “Studium der Reaktionskinetik Couple in Molten Fluorides,” Ana[. Chern. Diu. Ann. Progr. von Elektrodenvorgangen mit hilfe der Elektrolyse bei Konstan- Rept. Oct. 31, 1967, ORNL-4196, p. 23. tem Strom I. Studium der Dismutation der Ionen des Funfwert- ‘Analytical Instrumentation Group. igen Urans,” Collection Czech. Chem Commun. 24, 3046 120RAU Graduate Fellow from the Department of Chem- (1959). istry, University of Tennessee, Knoxville. 29

Table 3.3. Electrode Potentials in Molten Fluorides at 5OOOC

Couple Measured in Calculatedb in Standard State LiF-BeF2-ZrF4 LiF-BeF2 (65.6-29.4-510 mole %) (66-34 mole %Ic

Be/Be(II) -2.120 -2.168 LiF-BeF2 (66-34 mole %) Zr/Zr(IV) -1.742 -1.772 1 Mole fraction Cr/Cr(II) -0.754 -0.789 1 Mole fraction Fe/Fe(II) -0.408 -0.413 1 Mole fraction Ni/Ni(II) 0 0 1 Mole fraction

~ ~~~~ ~~~ =Values vs Ni/Ni(II) reference electrode. bPrivate communication with H. R. Bronstein, Chemistry Division. CValues converted to 500°C.

electrode potentials measured thus far. From a compari- (comparable with Bronstein’s tantalum frits). The frits son of the emf‘s in Table 3.3, it is believed that the will be fitted into copper tubes and tested for half-cell agreement between the measured values and those separation along with additional BN sheathes. If the calculated by Baes’ is reasonably good, even though penetration problem can be overcome, an attempt will the solvent systems were not the same. be made to obtain emf measurements on additional The Ni/NiF2 reference electrode consists of a thin- redox couples, including U(IV)/U(III), in molten LiF- walled (‘/3 2 -in.-thick) boron nitride (BN) compartment BeF2 -ZrF4. that contains the fluoride melt, NiF2 in a futed concentration, and a nickel electrode. Electrical contact 3.2.d Facility for Spectrophotometry of is made when the BN becomes wetted by the melt. Radioactive Samples Although the majority of the BN sheaths used thus far J. P. Young have been satisfactory, in a few cases the melt exten- sively penetrated the sheath. The reason for this The development of a spectrophotometric facility for behavior is not yet understood. The extent of penetra- hot-cell use has continued.I6 The scope of the project tion appears to be related to the free oxide content of has broadened somewhat. The facility will make use of the fluoride melts as well as to the previous history of an extended double-beam arrangement; both sample the BN (e.g., grade and amount of exposure to and reference beams will pass into and out of the hot atmospheric moisture during machining). Therefore, it cell. The conceptual optical design of the extended light was decided to seek other ways to separate the beams has been completed by Cary Instruments, half-cells. Monrovia, Calif., but a contract for its detail design and H. R. Bronstein’ successfully used tantalum construction has not. The spectrophotometer itself will sheathes with tantalum frits for half-cell separation in be outside the cell. The facility can be used with solid, chloride melts for several hours without significant liquid, or gaseous samples at temperatures up to diffusion. It seemed worthwhile to investigate this -800°C. As pointed out previously,’ the facility is approach for fluoride melts. C. J. King’ fabricated for designed primarily for use with molten-fluoride salts us copper frits (-3/,-in.-OD by ‘&-in. thickness) with a and will be used to demonstrate the spectrophotometric pore radius of -1 1.1 and a void fraction of -0.30 determination of U(II1) in molten-salt reactor (MSR) fuels (e.g., LiF-BeF-ZrF4-UF4), which contain U(1V). The spectrum of U(V) in molten-fluoride salts has I3C. F. Baes, Jr., “The Chemistry and Thermodynamics of Molten-Salt-Reactor Fluoride Solutions,” pp. 409-433 in voi. 1 recently been characterized (Sect. 3.2.e); it is now of Thermodynamics, International Atomic Energy Agency, Vienna, 1966.

^A I4Private communication with H. R. Bronstein, Chemistry 6J. P. Young, “Spectrophotometric Studies of Molten-Salt Division. Systems,” Anal. Chem Div. Ann. Progr. Rept. Oct. 31, 1967, ”Oak Ridge Gaseous Diffusion Plant. ORNL-4196, p. 25. 30

n possible to identify U(V) in MSR salt if it is present in handling, and maintenance can be carried out properly. at least 1000-ppm concentration. The obvious applicability of this installation to other Equipment has been designed and techniques are types of samples is also being considered in this design being developed to take a sample of fuel from the work. MSRE reactor, divide it into as many as five portions, For initial spectra analysis in this facility, the molten and transfer each of the portions to a spectrophoto- fluoride sample will be contained in a modified captive- metric furnace assembly without exposing the portion liquid cell’ adapted for remote-handling techniques. to the atmosphere or to temperatures below 200°C for However, the system is sufficiently versatile that it will periods longer than 0.5 hr. Exclusion of air is necessary accept other types of optical cells which are now being to prevent the reaction of U(II1) with H2 0 and/or 02. developed to contain molten salts, for example, the Elevated temperature is required to prevent the radi- diamond-windowed cell (Sect. 3.2.0. olytic evolution of fluorine, which occurs if the sample is allowed to remain at temperatures below -200°C for 3.2.e Spectral Studies of Uranium(V) and a long time. With evolution of fluorine, the oxidation Uranium(VI) in Molten Liz BeF4 state of uranium would most likely change on remelting J. P. Young the sample. The apparatus required for this sample transfer has The spectra of uranium in its higher oxidation states, been designed with the assistance of F. L. Hannon” that is, >U(IV), in molten Li2BeF4 have been studied and E. F. Marguerat.17 It consists of six components: further in collaboration with G. I. Cathers: who (1) Sample ladle, which removes a 5-g molten-salt supplied the solute Naz UF8 (UF6 adsorbed on NaF). It sample from the pump bowl of the reactor. (2) was found that Na2 UFs undergoes a rapid and vigorous Transport container, which receives the sample ladle reaction when placed in molten Liz BeF4 that is held in and maintains it under inert gas. (3) Heated transfer a graphite windowless container. Since gas is evolved in carrier, which receives the transport container, provides the process, it is assumed that Na2UF8 oxidizes a radiation shielding during transfer of the sample from portion of the graphite container. The spectrum of the F reactor to the hot cell, and heats the sample to -2OOOC colorless solution that results from this reaction is that during the transfer. (4) Sample-loading furnace, which of U(V); it consists of two overlapping peaks centered receives the transport container in the hot cell. Within at 950 and 1240 nm and a sharp peak at 1465 nm. The this assembly the 5-g sample is melted, and test portions corresponding molar absorptives (E’S) are -6,3, and 15 are transferred into as many as five containers for liters mole-’ cm-’ , respectively. They were calculated spectrophotometric study. (5) Spectrophotometric fur- by determining the decrease in absorbance of U(V) for nace lid, which fits both the sample-loading and a given increase in absorbance of U(IV). The U(V) spectrophotometric furnaces; the lids receive the spec- species is not stable in molten Li2BeF4 at 550°C; it tral sample for transfer between the two furnaces. (6) slowly disappears, apparently by disproportionation. Spectrophotometric furnace, which receives the sample From the spectral study, the rate constant for the for melting and spectral study. disproportionation of U(V) in molten Li2BeF4 was All the sample-handling operations must, of course, calculated to be 0.005 liter mole-’ sec-’ , a rate that is be carried out with manipulators behind suitable several orders of magnitude slower than that measured shielding. The apparatus is designed in such a way that in an electrochemical study of U(IV) oxidation.’ The the manipulations required at this reactor site fall large discrepancy between the two values is real and can within their routine procedure requirements. At the hot be explained if one assumes that the rate obtained in cell, the apparatus can be operated and general mainte- the electrochemical study is the result of catalysis at the nance can be done with master-slave manipulators. All surface of the electrode, whereas the spectrally re- these components except the sample-loading furnace corded rate is the rate for a noncatalyzed reaction in have been designed completely; components 1, 2, 5, bulk solution. and 6 are presently being fabricated for testing prior to The spectra of solutions of Na2UF8 in molten hot-cell use. Li2BeF4 contained in a windowless LaF3 cell were The optimum orientation of apparatus within the hot studied; LaF3 is slightly soluble in the solvent but cell is being determined so that all operations, sample

J. P. Young, “Spectra of Uranium(1V) and Uranium(II1) in ’7General Engineering Division. Molten Fluoride Solvents,”Znorg. Chem 6, 1486 (1967). 31

should not be oxidized by U(VI). No reaction was surface tension and general nonwetting properties of observed in this melt, unlike the case in graphite. The many molten fluoride salts, which prevent these liquids spectra of the resultant solutions showed strong absorp from flowing out of small openings. Since there is no tion in the ultraviolet region with shoulders near 270 need for elaborate window seals, the design of a and 315 nm. Some contamination of the solution with windowed cell can be relatively simple. Also, this - U(IV) and U(V) was evident from the spectra and arrangement decreases the probability of breaking these apparently was caused by reaction of U(VI) with thin windows during an assembly operation. As pres- ,.\ ,.\ impurities in the melt. It is assumed that the spectra ently constructed and used, the cell is not suitable for seen were those of U(VI) in some form of UF;-”. The highly radioactive samples; however, cells of later absorbing species is not UOz’+, which has been ob- designs may be. served in other studies.’ 3.2.g Absorption Spectra of Several 3d 3.2.f Containers for Molten Fluoride Salts Transition-Metal Ions in Molten Fluoride Solution J. P. Young J. P. Young The use of silica containers for molten fluoride salts has been reported.” As pointed out, the compatibility Experimental work has been completed on a spectral study of Fe(II), Ni(II), of silica with each component of a particular solution Cr(II), and Cr(lI1) in various molten fluoride salts. The results have been presented must be considered. Such things as oxide solubility and orally’ and submitted for publication: the abstract silicate formation can influence a system that may ’ from the manuscript follows: appear to be thermodynamically stable with respect to “The spectra of several 3d transition metal ions, Fe(II), Ni(II), the simple reaction Cr(II), and Cr(II1) have been studied; these ions were dissolved in several molten fluoride salts which are essentially the 4F- + Si02 =+SiF4 f + 202-. (3.1) stoichiometric mixture LizBeF4 with and without excess F-, as LiF. The spectra were obtained in the temperature range of T For example, it has been observed that solutions of 540°C to 650°C; the samples were contained in graphite Ni(I1) and of Co(I1) in molten Li2BeF4 cannot be windowless containers for the study. Fe(I1) exhibits a peak and maintained in a silica cell. Presumably, the low solu- shoulder absorbance envelope with maximum absorbance at bility of NiO and of COO results in the loss of these ions 9800 and 5500 cm-’. Respective molar absorptivities are 4.5 by brecipitation as oxide. The 0’- level is maintained and 3. The spectrum appears unaffected by change in solvent composition. The spectrum of Ni(I1) at a temperature of 550°C by the equilibrium indicated by Eq. (3.1). consists of 3 peaks at 23,100, 10,800 and ca 6000 cm-’. In cooperation with L. M. Toth’ and G. P. Smith,’ ’ Respective molar absorptivities are 11, 2, and ca 1. The a diamond-windowed spectrophotometric cell is being spectrum appears to be likewise unaffected by solvent change. developed for use with molten fluoride salts. In At a temperature of 55OoC,Cr(I1) appears to exhibit one peak at 14,000 cm-’ with a molar absorptivity of 6;Cr(II1) exhibits preliminary spectral studies, the prototype cell has been 3 peaks at 33,000, 22,600, and 14,500 cm-’ ; respective molar entirely compatible with solutions of Pr(II1) or U(IV) in absorptivities are cu 10, 10, and 7. The spectral results would molten Li2BeF4 maintained at temperatures as high as suggest that these ions are situated in Oh symmetry in these 550°C. Fluoride melts have not been permitted to melts with little tendency to change if the “free” fluoride ion solidify between the windows. Instead, prior to the concentration is reduced over the range studied. Fe(I1) is a possible exception to this generality.” cooling of a sample, the furnace and cell have been inverted so that the salt flows away from the windows; 3.2.h Spectrum of MoF3 in LizBeF4 thus, cleaning of the cell is facilitated. The cell is constructed of a graphite body and type I1 A diamond J. P. Young windows (about 5 X 5 X 1 mm). The windows are not In cooperation with L. M. Toth’ and G. P. Smith,’ ’ sealed to the cell body; rather, they are merely retained the spectrum of MoF3 in molten Li2BeF4 has been against it. This type of construction exploits the high

”J. P. Young, “Absorption Spectra of Several Transition ”C. E. Bamberger, J. P. Young, and C. F. Baes, Jr., Metal Ions in Molten Fluoride Solution,” presented at the “Containment of Molten Fluorides in Silica; Effect of Tempera- 155th National Meeting, American Chemical Society, San ture on the Spectrum of U4+ in Molten LiF-BeF2 Mixtures,” J. Francisco, Calif., Mar. 31-Apr. 5, 1968. Inorg. Nucl. Chem 30, 1979 (1968). 23J. P. Young, “Absorption Spectra of Several 3d Transition 20Reactor Chemistry Division. Metal Ions in Molten Fluoride Solution,” submitted for Metals and Ceramics Division. publication in Inorganic Chemishy. 32

studied. The spectrum of Mo(II1) in molten Li2BeF4 The pyrolytic-graphite electrode is not passivated by consists of two peaks at 353 and 472 nm; the E’S are -8 the addition of OH- or H20 to molten LiF-NaF-KF. and -12 liters mole-’ cm-’ respectively. This The 02- wave is seen easily at t0.8 V vs a platinum spectrum is consistent with the existence of Mo(II1) in quasi-reference electrode. Hydrogen is liberated from octahedral symmetry in molten Liz BeF4. These studies water at -0.45 V. The liberation of H2 from HF is seen have been carried out in windowless cells of graphite, at 0 V in a heavily contaminated melt. The above- # platinum, molybdenum, and copper. In all these cells, mentioned anodic and cathodic processes in molten Mo(II1) was lost completely. In the case of the graphite LiF-NaF-KF correspond well with the results obtained container, a thin film of molybdenum metal (-30 p by Pizzini and Morlotti.2 thick) was identified by electron-probe analysis. With The reduction of Ta(V) to Ta(0) in molten LiF- copper containers it is possible that the Mo(II1) is NaF-KF at a platinum electrode appears to be at least a reduced by hydrogen that diffuses out of the copper, two-step process, as reported by Senderoff, Mellors, and since all the copper containers were H2-fired prior to Reinhart.’ Our attempts to verify the reported oxida- use. tion of Ta(V) to Ta(VI) in molten LiF-NaF-KF’ have been inconclusive. 3.2.i Simultaneous Electrochemical The anodic dissolution of a copper electrode in and Spectrophotometric Study of Solutes molten LiF-NaF-KF produces oxidized copper in at in Molten Fluoride Salts least two oxidation states. An insoluble form of Cu(1) is F. L. Whiting24 J. P. Young produced at t1.1 V vs the platinum quasi-reference Gleb Mamantov7 electrode. A soluble form of Cu(I1) is believed to be produced at +1.35 V. The spectrum of Cu(1I) in molten The study of the electrochemical generation and LiF-NaF-KF consists of a band at 810 nm and an spectral identification of solute species in molten unresolved charge-transfer band in the ultraviolet fluoride salts has continued.21 It has been apparent region. The spectrum was obtained during the electro- that melt impurities, primarily hydrolysis products, chemical generation of Cu(I1) and was checked quali- must be absent if the desired solute species is generated. tatively by observing the spectrum of molten LiF-NaF- Various methods to purify LiF-NaF-KF have been KF to which CuF2 had been added. attempted. These have included treatment with HF and with SiF4 and a vacuum pretreatment at 450°C;25 the 3.3 NUCLEAR SAFETY vacuum pretreatment proved to be the most fruitul. The removal of HF from molten LiF-NaF-KF was 3.3.a Analysis of Purge Gas achieved best by evacuating the melt at 860°C whereas from In-Reactor Tests the SiF4 was removed at 500°C; SiF4 is highly soluble of Reactor Fuel Elements in molten LiF-NaF-KF, and its dissolution is an endothermic process. An increase in pressure and the C. M. Boyd W. F. Peed’ A. S. Meyer forms of the voltammograms of the melt indicated that A General Electric Company’s Monopole 600 Resid- HF and SiF4 had been removed at the temperatures ual Gas Analyzer (RGA) was acquired for the in-line cited. analysis of the gases generated by in-reactor tests of fuel A platinum- (10%) electrode is apparently elements. To adapt the RGA to the continuous mon- passivated by large additions of LiOH and/or H2 0. The itoring of the purge gas, a small fraction of the effluent passivation results in the elimination of voltammograms stream will be bled at 1 to 10 torr into an intermediate- that occur anodically with respect to the reduction of pressure system located in a shielded hood at the ORR. OH-. Thus, with platinum electrodes, it would be difficult to distinguish between a very contaminated 26S. Pizzini and R. Morlotti, “Oxygen and Hydrogen Elec- and a clean melt. trodes in Molten Fluorides,” Electrochim Acta 10, 1033 (1965). 27S. Senderoff, G. W. Mellors, and W. J. Reinhart, “The 24Student Guest from the Department of Chemistry, Uni- Electrodeposition of Coherent Deposits of Refractory Metals. versity of Tennessee, Knoxville. 11. The Electrode Reactions in the Deposition of Tantalum,” J. Electrochem SOC. 112,840 (1965). 25S. pizzini, R. Morlotti, and E. Romer, “Electrode Over- voltages in Molten Fluoride - The Anodic Behavior of Nickel ”G. W. Mellors and S. Senderoff, “Hexavalent Fluorides of Electrodes in Fluoride Melts,” J. Electrochem SOC. 113, 1305 Tantalum and ,”J. Electrochem SOC. 112,642 (1965). (1966). 290nloan from Thermonuclear Division. 33

By way of a capillary, a sample will be withdrawn Tests were made on the pumping speed of the continuously from the intermediate-pressure system 250-liters/sec ion pump; the speed was found to be and injected into the ionizer section of the RGA to give -200 liters/sec for nitrogen and 20 liters/sec for a pressure in the analyzer of the order of 10-6 torr. Ths helium. Difficulties were encountered in reducing the system has been assembled in the laboratory for testing background that was caused by moisture and hydro- and calibration. A thermostatically controlled oven and carbons in the system. The automatic gate valve, which facilities for heating the ion pump, sample lines, and all contained Viton O-rings and was located between the parts of the high-vacuum system are included. analyzer and the ion pump, was removed. This change Since some of the in-reactor tests will require the resulted in a substantial decrease in the background. exposure of the fuel elements to air, the effect of air Engineers from the General Electric Company are samples on the RGA was checked. It was found that now investigating the cause of an electronic malfunc- exposure to air at torr adversely affects the tion that produces an interaction between the electron- analyzer. Some components of the analyzer tube, emission current and the ion-energy adjustment. particularly the electron-accelerating grid, are oxidized. A second electronic problem is the loss of the low end This effect causes poor peak shapes and a loss of of the mass scan range; this loss interferes with the adequate resolution. The analyzer tube was returned to observation of masses 1 through 4. Adequate resolution the General Electric Company for gold plating of the of the lower-mass ranges depends on the selection of metal components. This gold plating greatly improved the feedback-rectifier tube (6AL.5). Even the more the resistance of the analyzer to the effects of air. Only effective tubes are degraded during scans of the slight changes in resolution and peak shape were higher-mass range (i.e., >200). The Vacuum Products observed after exposure to air at torr for 2 hr at Division of the General Electric Company is attempting 200OC. to modify the circuit to reduce the loading of this tube. .

4. Analytical Biochemistry

Gerald Goldstein

4.1 MACROMOLECULAR SEPARATIONS ATP 1 micromole PROGRAM K+ 1.25 micromoles Enzyme 10 to 50 pg of protein 4.1 .a Determination of TyrosincAccepting Transfer Ribonucleic Acid (tRNAfy*) The volume of the assay solution is 0.25 ml, and the incubation time is 30 min at 37OC, although amino- I. B. Rubin acylation is complete in 20 min for this range of protein The optimum conditions for the determination of quantity. A reducing agent is not necessary, but 2.5 picomole quantities of tyrosine-accepting transfer ribo- micromoles of 2-mercaptoethanol is added with the nucleic acid (tRNAtyr) have been established. The enzyme. Under these conditions, aminoacylation is procedures used for studies of this nature have been linear over the minimum range 4 to 80 picomoles of described.’ The conditions that result in maximum tFiNAtYr. aminoacylation are:

PH 8.2 ‘I. B. Rubin, A. D. Kelmers, and G. Goldstein, “The Buffer Cacodylic acid, 25 micromoles Determination of Transfer Ribonucleic Acid by Aminoacyla- Tyrosine-14C 375 picomoles tion. I. Leucine and Phenylalanine Transfer Ribonucleic Acid MgB 2.5 micromoles from E. Coli B,”AnaL Biochern 20,533 (1967). 34

4.1.b Determination of Methionine-Accepting The second stage of the program will consist in testing Transfer Ribonucleic Acid (tRNAmef) those variables whose effects could not be definitely established from the results of the screening test. This D. W. Hatcher stage for the tRNAtyr study has been planned; it Partially purified methionine-accepting transfer ribo- consists in testing five variables in 28 assays. It is nucleic acid (tRNA"") is now being prepared by the estimated that a complete study for a given tRNA will Chemical Technology Division. The optimum condi- take less than ten man-days of laboratory work as tions for its determination were established. The tech- compared with the 30 or more usually needed by the niques used have been described previously.' The conventional system. The estimated ten days does not following conditions were found to be optimum: include the time needed for analysis of each set of results and for preparation of the next step of the tRNA 0.01 to 0.03 ODU program. Methionine-14C 1000 picomoles PH 8.0 4.1 .d Automated Determination of Transfer Buffer HEPES, 50 micromoles Ribonucleic Acids (tRNA's) ATP 2 micromoles Mg2+ 5 micromoles Gerald Goldstein W. L. Maddox3 I. B. Rubin Glutathione or p-mercaptoethanol 5 micromoles Aminoacyl-tRNA synthetase 90 fig of protein A modified version of the automated tRNA analyzer Incubation time 30 min described last year4 was designed, constructed, and 3OoC Incubation temperature tested and is now in routine operation. Two major changes were made. By the use of micro tubing on the These conditions are required for an assay volume of proportioning-pump manifold, the volume of reagents 0.5 ml. consumed was reduced by -30%. The stream-sampling mechanism, which in the previous model was activated 4.l.c A Fractional Factorial Method for by detection of a dye with a flow colorimeter, is now . Optimizing Conditions for the Determination keyed directly to the Technicon Sampler. Further of Transfer Ribonucleic Acid (tRNA) details about the modified analyzer are given in Sect. I. B. Rubin 1.10. The precision and accuracy of the assays are essentially unchanged. A statistical approach for establishing optimum condi- tions for the determination of specific tRNA's has been 4.1.e Computer Processing of Liquid- designed by T. J. MitcheL2 This scheme is the Scintillation-Counting Data in the Analysis fractional factorial method. It is designed to test of Transfer Ribonucleic Acids (tRNA's) simultaneously a maximum number of variables with a minimum number of assays. The first, or screening, step Gerald Goldstein has been carried out on three purified tRNA materials; With >50,000 tRNA assays per year now being tyrosine-, lysine-, and glutamic acid-accepting tRNA's reported, both the Analytical Chemistry and Chemical (tRNAtyr, tRNA1yS, and tRNAglU). The optimum con- Technology Divisions have been compelled to spend ditions for determining the tRNAtYr have already been considerable time in transcribing liquid-scintillation- established by conventional means, that is, by testing counting data, making calculations to tRNA concen- one variable at a time (Sect. 4.1.a). The screening step trations, and plotting. We have now acquired a key- consists in testing nine variables in only 32 assays. punch adapter and an IBM key punch for one of our These variables are: (1) time, three incubation periods; liquid-scintillation counters so that the data are re- (2) two buffers; (3) pH, three values; (4) amino corded directly on punched cards. A computer program acid-' C, three concentrations; (5) ATP, three concen- has been written that provides two forms of readout: trations; (6) Mg2+, three concentrations; (7) enzyme, three concentrations; (8) K'and NH4+, three concentra- tions each; and (9) two reducing agents, three concen- 3Analytical Instrumentation Group. trations each. - 4G. Goldstein, W. L. Maddox, and I. B. Rubin, "Automated Determination of Transfer Ribonucleic Acids (tRNA's),'' Anal. Chem Div. Ann. Progr. Rept. Oct. 31, 1967, ORNL4196, p. Mathematics Division. 46.

-. 3s

ORNL-DWG. 68-12477

0 ILE 4 o PHE

+ MET E x VAL

!

11

1

r.

+

i I c 0 20 4

Fig. 4.1. Computer Plot of tRNA Chromatograms.

(1) a printed tabulation of the sample identification, 4.1.f Kinetics of Aminoacylation of Transfer counting data, picomoles of tRNA, and running sum of Ribonucleic Acid (tRNA) the total tRNA recovery and (2) a plot of picomoles of D. W. Hatcher tRNA found vs chromatographic fraction number. Chromatograms for as many as ten different tRNA’s Observed effects of temperature on tRNA assays have can be plotted on a single grid; Fig. 4.1 is a typical plot. suggested to us that the degree of aminoacylation of We are now in the process of acquiring an adapter and tRNA, under a given set of conditions, is described best key punch for a second counter. The second key punch as a steady-state concentration in a dynamic equilib- will also be capable of converting punched-paper tape rium. For example, Fig. 4.2 shows the effect of -. - to cards. When the Chemical Technology Division temperature on the aminoacylation of phenylalanine- installs punched-tape readouts for their spectropho- accepting tRNA (tRNAphe). An increase in tempera- tometer, we will process optical and counting data ture causes an increase in the initial rate of aminoacyla- together. tion but not necessarily in the equilibrium 36

ORNL-DWG. 58-12 ORNL-DWG. 68-709 I I 1 I

600

500

400

3 00

200

100

I I I I I > 40°C 0 10 20 30 40 50 60 10 20 30 40 50 60 TIME, rnin HYDROLYSIS TIME , rnin

Fig. 4.2. Effect of Temperature on the Aminoacylation of Fig. 4.3. Kinetics of Hydrolysis of PhenyhIanheAccepting tRNAPhe. (tRNAPhe) (pH 8.4 ionic strength = 0.1).

concentration. This temperature effect is rapidly revers- velopment of an economical procedure for reclaiming * ible. We postulate a sequence of three reactions, all of the expensive amino acids-' 4C from their assay mix- which are known to occur, that result in a cyclic tures would realize a saving in both the manual and process as follows: automated procedures and make the automated pro- cedure even more attractive. k Extraction of the amino acid-14C from the assay aa E ATP (E-aa-AMP) + PPI , + + mixtures by anion- and cation-exchange resin columns k- 1 and by a liquid cation exchanger has been investigated. k The cation-exchange resin worked much better than the (E-aa-AMP) + tRNA tRNA-aa + AMP + E , k-2 anion-exchange resin. However, a large excess of con- centrated hydrochloric acid was required to remove the amino acid from the resin column, and no simple means tRNA-aa + H2 0 %tRNA + aa. could be found to separate the amino acid from the mineral acid. The liquid cation exchanger did not We are attempting to measure the individual reaction present this problem. rate constants, kl, k2,and k3. The liquid cation exchanger di(Zethylhexy1)- The rate of hydrolysis, k3,has been determined (Fig. orthophosphoric acid (HDEHP) dissolved in n-hexanol 4.3) and from this the heat of activation of the is used to extract the amino acids-14C from the assay hydrolysis was calculated to be 13.7 kcal/mole. mixture. By means of coarse sintered-glass filter tubes, a 10 v/v % HDEHP solution is allowed to percolate as 4.1.g Reclaiming Amino Acids-' C tiny droplets up through the solution that contains the D. W. Hatcher assay mixture and then through three consecutive dilute hydrochloric acid stripping solutions which remove the The procedure for determining tRNA's by aminoacyl- mino acids from the HDEHP. Figure 4.4 shows the ation with ' 4C-labeled amino acids has been automated apparatus. The assay mixture must be strongly buffered v (Sect. 4.1.d). A disadvantage of the automated pro- at pH 3.0 to 3.5 by use of a phosphate buffer, and the cedure is the increased consumption of amino acids-I4 C stripping stages must be at least 0.1 M in HCl. If one compared with that of manual assay. Therefore, de- recycles the organic solution through the system, only 37

ORNL-DWG. 68-12479 Ribonucleic Acid (RNA). - The conventional orcinol spectrophotometric method for RNA6 was found to be

40 v/v % HDEHP extremely sensitive to the presence of salts, buffers, and IN n -HEXANOL (UPPER PHASE) other reagents commonly used in the isolation of RNA. By increasing the concentration of HCI in the reaction mixture from 6.0 to 7.2 N and adding 0.5 ml of n-butanol most of these interferences are eliminated and the sensitivity is increased by 30% (Table 4.1). The recommended composition of the assay mixture is:

Component Volume (ml) Sample 1.0 Orcinol (4 g per 100 ml of ethanol) 0.5 Ferric chloride (2.5 g per 100 ml of concd HCI) 0.5 HCl (concd) 2.5 n-Butanol 0.5

From 10 to 800 pg of RNA can be determined with a relative standard deviation of -5%. Deoxyribonucleic Acid (DNA). - We find that the diphenylamine spectrophotometric method for DNA7 is severely influenced by the presence of salts, buffers, and other reagents used to separate RNA from E. coli B cells (Table 4.2). The indoleacetic acid procedure for DNA8 was rejected because it gave poor performance in evaluation tests. Fig. 4.4. Apparatus for Reclaiming Amino A~ids-’~C. Cadmium(I1) quantitatively precipitates DNA and does not interfere in the diphenylamine reaction. We are testing to see whether precipitation by Cd(1I) can be used to isolate DNA for its determination. An overnight dialysis of DNA samples does not eliminate alcohol, small volumes of both the organic and stripping phenol, or glutathione, which interfere in the diphenyl- solutions are required. amine reaction. This procedure has given 93% recovery of phenyl- Polysaccharide. - The enzymatic procedure for de- alanine-’ C from assay mixtures. The recovery of other termining free glucose’ can be used to determine amino acids looks just as promising. Additional work is polymeric glucose in tRNA samples after hydrolysis of necessary to establish the purity and specific activity of the polysaccharide. Heating for 20 min at 100°C in 2 N the reclaimed material. HCl gives complete hydrolysis of the soluble starch that we use as a polysaccharide standard. The pH of this 4.1.h Chemical Analysis of Transfer hydrolyzate is then adjusted to 7.0 0.5 before glucose Ribonucleic Acids (tRNA’s) is determined. No sample interferences have been D. W. Hatcher encountered, and glucose in concentration as small as 5 pg/d can be measured. For some time, we have been determining impurities in purified tRNA samples.’ Recent experience with highly impure materials, however, has indicated that 6G. L. Miller, R. H. Golder, and E. E. Miller, “Determination our methods are not adequate and require modification. of Pentoses,” Anal. Chem 23,903 (1951). The following improvements have been made. ‘K. Burton, “A Study of the Conditions and Mechanism of the Diphenylamine Reaction for the Colorimetric Estimation of Deoxyribonucleic Acid,” Biochem J. 62,315 (1956). ’G. Goldstein, “Determination of Impurities in Transfer 8P. Schmid, C. Schmid, and D. C. Brodie, “The Determi- Ribonucleic Acids (tRNA),” Anal. Chem Div. Ann Prop. nation of the Total Deoxyribose of Deoxyribonucleic Acid,” J. Rept. Oct. 31, 1966, ORNL4039, p. 40. BioL Chem 238, 1068 (1963). 38

Tabie 4.1. Effect of Composition of the Reaction Mixture on Interferences in the Orcinol Spectrophotometric Method for RNA

RNA Recovered (mg)b lnterference 6.0 N HCl, 7.2NHC1, 7.2NHC1, ldentity Ma No Butanol No Butanol Butanol Added

Na acetate 0.10 0.25 0.25 0.26 NaCl 0.10 0.27 0.24 0.25 MgCl2 0.10 0.24 0.26 0.26 CdCl2 0.10 0.20 0.26 0.26 Na2 s2 O3 0.05 (PPt) (PPt) (PPt) EDTA 0.012 0.17 0.26 0.25 Glutathione 0.005 0.14 0.22 0.22 lsopropanol 0.13 0.22 0.27 0.25 Phenol 0.093 0.14 0.15 0.20

aCalculated for assay mixture. b0.25 mg added.

Table 4.2. Interferences in the Diphenylamine 4.1 .i Terminal Nucleoside Assay of Ribonucleic Acid Spectrophotometric Method for DNA by Ligand-Exchange Chromatography

Substance Tested C. A. Burtis Gerald Goldstein Interference (%) ldentity Ma An article was published’ that describes the work on

Sodium acetate 0.18 - 23 the terminal nucleoside assay of ribonucleic acid by 0.30 -47 ligand-exchange chromatography; the summary from Tris buffer 0.01 -15 the article follows: Glutathione 0.001 -33 “The nucleosides released from polyribonucleosides and 0.01 -100 p-Mercaptoethanol RNA’s by alkaline hydrolysis may be identified and quantitated 0.005 -19 EDTA by ligand-exchange chromatography on a copper-loaded che- 0.01 +14 MgCl2 lating ion exchanger. With a suitably sensitive ultraviolet 0.05 +34 absorbance monitor and recorder, this analysis can be effected Phenol 0.09 -45 on as little as 10 nM of free nucleoisde in 1-2 hr with an HC104 0.2 -30 accuracy (standard deviation) of 3-476. Dephosphorylation Ethanol 1.7 -70 prior to alkaline hydrolysis allows the assay of ,nucleosides Glycine 0.4 -73 bearing primary phosphate residues in the 3 - (or 2 -) position. The method is useful in quantitating the nucleoside at the aCalculated for the assay mixture. aminoacyl-acceptingend of tRNA’s.”

Protein. - The spectrophotometric procedure of 4.1 .j Gel Electrophoresis of Ribonucleic Acid (RNA) Groves, Davis, and Sellsg has proven to be reliable for A. L. Travaglini determining protein concentrations. For nucleic acids, the difference in absorbances at 220 and 240 nm is Preliminary studies on electrophoresis of RNA were minimal, whereas for protein the difference is a linear begun. The particular RNA used, although thought to function of concentration. Thus, by use of carefully be pure, actually contained a large amount of a selected wavelengths at which the absorbances of fast-moving fraction and a small amount of a slow- nucleic acids are equal, we are measuring protein moving fraction. The staining and fining solution used concentrations in the range 5 to 180 pg/ml without was toluidine blue (0.01 w/v %)-trichloroacetic acid interference from nucleic acids. (10 v/v %)-lanthanum nitrate (0.1 M). Of those

c 9W. E. Groves, F. C. Davis, Jr., and B. H. Sells, “Spec- trophotometric Determination of Microgram Quantities of ‘OC. A. Burtis and G. Goldstein, “Terminal Nucleoside Assay Protein Without Nucleic Acid Interference,” Anal. Biochem 22, of Ribonucleic Acid by Ligand-Exchange Chromatography,” 195 (1968). Anal. Biochem 23,502 (1968). 39

studied, this was the only mixture of stain and faative possible interferences that may be present after the that is stable to electrophoretic destaining of the chromatographic separations, and automating the assay. background and that provides a medium in which the 5 dyed RNA bands do not diffuse during storage. More 4.1.1 Determination of Subnanomole Quantities of . study of the effects of buffers and pH on the separation L-Amino Acids by Isotope Dilution-Aminoacylation of RNA’s and on the sensitivity will be required. I. B. Rubin 4.1 .k Determination of L-Asparaginase A procedure is being developed for the determination I. B. Rubin of subnanomole quantities of specific L-amino acids. This procedure uses isotope dilution in conjunction It is anticipated that, in the near future, the Biology with the standard aminoacylation method for the and Chemical Technology Divisions will start a program determination of transfer ribonucleic acid (tRNA).’ to produce L-asparaginase. Consequently, a study has The unlabeled amino acid is added to the tRNA assay been initiated to develop a procedure for L-asparaginase solution of the same 14C-labeled amino acid. The (L-asparagine amidohydrolase EC 3.5.1.1) suitable for decrease in the count rate of an aliquot of the solution its routine determination in a large number of chro- is directly proportional to the quantity of unlabeled matographic fractions that would contain various quan- acid present. This method should be very useful for the tities of this enzyme. As a first step, the procedure of determination of amino acid concentrations in peptide Campbell and associates’ for determining the two hydrolysates that result from various biological stud- L-asparaginases from E. coli B has been coupled with ies.” The hydrolysates need only to be evaporated to Layton’s’ ’ spectrophotometric sodium phenate meth- remove the hydrochloric acid and then dissolved either od for the determination of ammonia. The quantity of in water or in Tris, cacodylate, or acetate buffer. No ammonia formed by the reaction derivatization of the amino acids is necessary, and only nanomole quantities of sample are needed. This proce- L-asparaginase L-asparagine + H2 0 > L-aspartate + NH3 dure should also be suitable for the determination of the L-component of DL-amino acid mixtures. is directly proportional to the amount of enzyme added To date, calibration data have been obtained for when the asparagine is present in excess and when the alanine, arginine, asparagine, aspartic acid, cystine, inchbation period is <30 min.” An aliquot of the glutamic acid, leucine, lysine, methionine, phen- assay solution is mixed directly with the chromogenic ylalanine, serine, tyrosine, and valine. In general, the reagents for the ammonia determination without pre- calibration curves are linear over the range 0 to 3 vious deproteinization of the assay solution. Tests with nanomoles of added unlabeled amino acid. However, pure L-asparaginase have indicated that the absorbance the calibration curve for alanine is linear only from 0.2 of the resulting chromophore varies linearly with the to 3 nanomoles, and that for cystine only up to 1.5 quantity of ammonia released by 0.03 to 0.18 unit of nanomoles. Cystine and cysteine cannot be distin- enzyme. A unit is that quantity of L-asparaginase that guished by this procedure. Relatively large quantities will release 1.0 micromole of ammonia per minute (>2 nanomoles) of asparagine and aspartic acid do under the conditions of the assay.’ interfere with the determination of smaller quantities of Future work will involve scaling the assay and the other. However, in hydrolysates that contain no chromogenic solutions to a smaller volume, studying asparagine, aspartic acid appears to assay as asparagine. This reaction may be caused by asparagine synthetase activity in the crude aminoacyl synthetase enzyme ’’H. A. Campbell, L. T. Mashburn, E. A. Boyse, and L. J. mixture. Old, “Two L-Asparaginases from Escherichia Coli B. Their The accuracy of this procedure is good, and there Separation, Purification, and Antitumor Activity,” Bie appears to be no bias. The precision also is good (S > chemistry 6, 721 (1967). ’F. L. Layton, “Ammonia, Spectrophotometric Sodium Phenate Method (Nitrogen),” Method Nos. 1 220020 and 9 14J. C. White, C. A. Horton, and I. B. Rubin, “Analytical 00720020 (9-25-62), OWL Master Analytical Manual, TID- Biochemistry,” Anal. Chem Div. Ann. Progr. Rept. Nov. 15, . 7015, Supplement 5 (1963). 1964, ORNL-3570, p. 29. 133.5.1.1 Asparaginase (E. Coli? (L-asparagine amdohy- lSJ. E. Attrill and R. A. Popp, “Amino-Acid Sequence drolase), Catalog from Worthington Biochemical Corp., Free- Analysis,” Anal. Chem. Div. Ann. Progr. Rept. Oct. 31, 1967, hold, N.J. (April 1967). ORNL-4196, p. 53. 40

Table 4.3. Comparison of Amino Acid Analyses If it is assumed that the copper on the column is of a Simulated Peptide Hydrolysate coordinated to only one ammonia molecule' which is replaced by one ligand molecule, the equilibrium for * Amino Added Found (micromole/ml) the replacement can be written Acid (micrornole/ml) This Worka Chromatographyb . L + -CU(NH~) -CU(L) + NH3 . ("3) 0.29 ASP 0.30 0.6 1 0.53 Also, Asn 0.30 0.59 I Leu 0.30 0.31 0.28 LY s 0.24 0.30 0.25 Met 0.30 0.33 0.30 Phe 0.30 0.29 0.27 Val 0.30 0.29 0.32 where Kf and KNH~refer to the formation constants of -Cu(L) and -Cu(NH3), respectively. Since =0.30- and 0.60-nanornole portions taken for analysis. bAnalyzed by J. E. Attrill. (-CW 1 Kd a PI 10%). The data of Table 4.3 show that the results then compare well with those obtained by chromatographic analysis with an amino acid analyzer. ["3 1 Kf Future work will involve obtaining calibration data Kd a- for the remaining amino acids, applying this procedure (-Cu("3)) KNH3 ' to actual peptide hydrolysates, resolving the anomalous situation with asparagine and aspartic acid, and ap- and, if constant terms are left out, then plying this procedure to racemic mixtures of amino a acid.

4.2 LIGAND-EXCHANGE CHROMATOGRAPHY It is well known17 that the formation constants of metal-ion complexes which have a series of structurally 4.2.a Principles of Ligand-Exchange Chromatography similar ligands, in solution, are related to the basicity of on Copper-Loaded Chelex Resin Columns the ligand by Gerald Goldstein From the chemical equilibria involved and several (4.4) simplifying assumptions, a simple relationship can be derived between the basicity of a compound and its If we assume that this trend is true, even when the retention volume on a column of copper-loaded Chelex metal is sorbed on a resin, then by combining Eqs. resin. (4.2), (4.3), and (4.4) Retention volume (V,) on a column is related to the ratio (Kd)of the distribution of the material between VA [NH,] a- 1 the column and the aqueous phases by the equation Ka or

log VA a pKa - log [NH,] . where Vo is the void volume and W is the weight of (4.5) resin if Kd is independent of the concentration of the material (linear isotherm). It follows that on a column 6K. Shimornura, L. Dickson, and H. F. Walton, "Separation of a given W of Amines by Ligand Exchange. Part IV. Ligand Exchange with Chelating Resins and Cellulosic Exchangers," Anal. Chim Acta 37,102 (1967). . 7A. E. Martell and M. Calvin, Chemistry of the Metal Chelate Compounds, p. 151, Prentice-Hall, Englewood Cliffs, N.J., where VA is the corrected retention volume. 1952. 41

Table 4.4. Retention Volumes and pK, Values ORNL- DWG. 68- 12480 of Some Uracil Derivatives jo.0 I I I I Compound PKa" VA (ml) log vi

Pseudouridine 8.97 10.5 1.02 Deoxyuridine (9.1) 12.3 1.09 Uridine 9.17 12.9 1.11 Uracil 9.45 17.4 1.24 Thymidine 9.65 20.8 1.32 5-Methyluridine (9.7) 22.1 1.34 9.5 Thymine 9.9 26.9 1.43 Dihydrouridine (10.0) 29.6 1.47 kb Q aValues in parentheses are not listed in the literature but are estimated from this work.

The relationship of Eq. (4.5) was tested with a series of uracil derivatives on a 60- by 0.9-cm column; the eluent 9 .O was N NH40H at a flow rate of 0.78 ml/min. Uridylic acid was added as a void-volume marker, because it is not retained on the column. Table 4.4 and Fig. 4.5 show the results. The agreement between the 1.0 1 .I 1.2 1.3 1.4 1.5 experimental results and the theory is very good; Eq. LOG VR' (4.5) enables us to predict from known PKa values whether separations are feasible or not. Fig. 4.5, Relationship Between pKa and Retention Volumes of Uracil Derivatives. 4.2.b Separation of Compounds of Biological Interest by Ligand-Exchange Chromatography tests indicate that the thionucleosides are, indeed, Gerald Goldstein J. C. Wolford' retained on a column and that separations may be possible. We have shown previously that ribonucleosides can be separated by chromatography on a copper-loaded che- lating resin.' We find that the deoxyribonucleosides 4.3 MOLECULAR ANATOMY PROGRAM can also be separated and that each except deoxyuri- 4.3.a Identification of Urinary Constituents dine can be distinguished from the corresponding Isolated by Anion-Exchange Chromatography ribonucleoside (Fig. 4.6). We are currently testing the separation of xanthine C. A. Burtis Sidney Katz2' and its methylated derivatives. These compounds are High-pressure anion-exchange chromatography of similar in structure to the purine bases found in nucleic urine has resolved more than 100 ultraviolet-absorbing acids and are natural products of biological interest. urinary constituents. Two methods have been used to Figure 4.7 shows the separation of caffeine (1,3,7- identify them: (1) comparison of the chromatographic trimethylxanthine), theobromine (3,7-dimethyl- properties of reference compounds with those of the xanthine), and theophylline ( Iy3-dimethylxanthine). urinary constituents (tentative identification) and (2) Since sulfur forms strong bonds with copper, we are spectrometric analysis of isolated urinary constituents examining the possibility of separating sulfur-containing through identification. compounds on copper-loaded columns. Preliminary In the first approach, reference solutions of biochemi- cals known to be in urine were chromatographed by .. .. 18Student Guest from the Department of Chemistry, Uni- versity of Tennessee, Knoxville. '9G. Goldstein, "Ligant-Exchange Chromatography of Nucle- otides, Nucleosides, and Nucleic Acid Bases," Anal. Biochem 20,477 (1967). 20Chemical Technology Division. 42

ORNL-DWG. 68-!248

Column: copper-loaded Chelex-100, 60 by 1 cm Urd d U rd Eluent : I N NH40H at 0.5ml/min

0 WN a

4 3 2 I 0 TIME, hr

Fig. 4.6. Separation of Rib@ and Deoxyribonucleosides by Ligand-ExchangeChromatography.

OR N L- DWG. 68-12482 anion-exchange chromatography.2 72 The column ef- I I fluent was collected, and the ultraviolet (W) spectivm Column : copper-loaded Chelex, 60 x Icm of the effluent associated with each of the separate Eluent : 3 N NHdOH at 1.4 ml/ min peaks was determined and compared with the UV spectra of the reference compounds. From either this THEOBROMINE comparison or absorbance ratios at two or more n wavelengths, the chromatographic positions of the reference chemicals were established. In instances where the chemical had little or no UV absorbance, I4C- 0 isomers of the compounds were chromatographed, and W N a their chromatographic positions were determined by monitoring the column effluent for radioactivity. The elution volumes of 1 12 urinary compounds are given in Table 4.5. Urine samples were chromatographed with and without the above-mentioned chemicals. By com- parison, ten of the urine components were tentatively

I I 90 60 30 , 21C. D. Scott, J. E. Attrill, and N. G. Anderson, “Automatic, High-Resolution Analysis of Urine for Its Ultraviolet Absorbing TIME, min Constituents,”Proc. SOC.Exptl. Biol. Med. 125, 181 (1967). 22C. A. Burtis and K. S. Warren, “Identification of Urinary Constituents Isolated by Anion Exchange Chromatography,” -- Fig. 4.7. Separation of Xanthine Derivatives by Ligand- Exchange Chromatography. Clin. Chem 14, 290 (1968). 43

Table 4.5. Elution Volumes of Known Urinary Biochemicals Separated by Anion-Exchange Chromatography”

~ Compound Elution Volumeb (ml) Compound Elution Volumeb (ml)

Adrenaline 14c Glutamic acid 22s Arginine 14 &Methyladenine 240 Cyanocobolin 14 Guanine 24 1 Cystine 14 Aspartic acid 270 3,4-Dimethoxyphenylethylamine 14 Urocanic acidd 381 Dopamine 14 Estratriol- 16~Y-glucuronide 428 Histidine 14 Uric acidd 550 Lysine 14 Nicotinuric acid 569 Metanephrine 14 Nicotinic acid 581 3-Methoxytyramine 14 Indoleacetamide 598 Noradrenaline 14 Phenol 636 Normetanephrine 14 Maleuric acid 650 Thiamine 14 Estratriol-3-glucuronide 721 Serotonin 14 Testosterone glucuronide 807 pTyramine 14 Hippuric acidd 817 Asparagine 18 Citric acid 820 Citrulline 18 pAminobenzoic acid 863 Creatine 18 3-Methoxy4hydroxymandelic acid 871 Glutamine 18 Estratriol-17a-glucuronide 876 Glucose 18 Quinaldic acid 914 Trigonelline 18 Homovanillic acid 916 Creatinined 19 Syringic acid 975 Cytosine 20 pHydroxyphenyllactic acid 1010 Alanine 21 pHydrox ymandelic acid 1019 Ergothioneined 21 pHydroxyphenylacetic acid 1020 Methionine 21 Anthranilic acid 1064 Proline 21 Benzoic acidd 1073 Urea 21 3-Indoleacetic acid 1106 Cytidine 24 5-Hydroxyindoleacetic acid 1114 Deoxycytidine 25 m-Hydroxyphenylacetic acid 1125 N-A cetyltryptophan 25 Vanillic acid 1156 Pyridoxal 2s Phloretic acid 1194 Pyridoxine 25 Estrone sulfate 1210 Phenylalanine 27 Folic acid 1212 Tryptamine 27 Kynurenic acidd 1214 Pseudouridined 29 o-Hydroxyhippuric acid 1253 Uridine 38 >Indoleglycolic acid 1266 Deoxyuridine 39 Salicylacetic acid 1272 Theobromine 39 3-Hydroxyanthranilic acid 1287 UlXCil 42 Aconitic acid 1297 Nicotinamide 42 m-Hydroxybenzoic acid 1343 Thymidine 45 pHydrox ybenzoic acid 1349 N-Methylnicotinamide 47 &Hydroxybenzoic acid 1350 Tyrosine 49 3-Methoxy-4-hydroxycinnamic acid 1390 Caffeine 50 Homogentisic acid 1417 Deox yinosine 62 a-Resorcylic acid 1430 4-Amines-imidocarboxamide 72 Indoleacrylic acid 1440 Hypoxanthined 85 p-Hydroxycinnamic acid 1443 Riboflavin 92 Xanthurenic acid >lSOO Deoxyadenosine 94 Adenosine 101 ‘Chromatography was performed with a 0.45- by 200-cm Tryptophan 110 stainless-:tee1 column; 5- to 10-p Dowex 1-X8 resin; tempera- ture, 40 C for 16 and 6OoC for 16 to 48 operating 5) 1-Methylguanine 118 hr hr; 7-Methylguanine 120 pressure, 1000 to 2000 psig; eluent, sodium acetate-acetic acid Theophylline 137 buffer at pH 4.4, varying in concentration from 0.015 to 6 M; >Hydroxykynurenine 146 and average flow rate of eluent, 28 to 30 ml/hr. ’A Adenine 152 bNumbers represent the average of three or more determi- Xanthosine 163 nations with a relative standard error of +1 to f3%. Xanthined 172 cColumn breakthrough. Guanosine 214 dTentatively identified in a urine chromatogram. 44 identified. The other compounds were either present at mass spectrometry (MS), infrared (IR), nuclear mag- concentrations below our detection limits or, because netic resonance (NMR), and UV spectroscopy and of chemical conjugation, were eluted at a volume interpretation of the resultant spectra. This approach different from that of the reference chemical. was used to identify as hippuric acid the component The spectrometric analysis entails separation of the eluting at a column volume of 817 ml. Sodium urinary constituent by gel chromatography followed by hippurate was separated from the acetate buffer (Fig. 4.8) and analyzed by MS and NMR. The resultant spectra were compared with the MS (Fig. 4.9) and NMR ORNL-DWG. 67-1168 I I I I I I I I I (Fig. 4.10) spectra of reference hippuric acid. Because Chromatographic Conditions : the MS and NMR spectra of the urinary component and Column, 2.5 x lOOcm hippuric acid match, the analyses indicate that hippuric Resin, G-10 Eluent, distilled water, 25°C acid was contained in the eluate at 8 17 ml. Flow, 2.2 ml /min Sample, hippuric acid peak from prep Dowex I-8X column 0.5 ' j105 STANDARD HIPPURIC ACID Y HIPPURIC ACID PEAK a- FROM COLUMN W a 60 - W 03- a 40- LL 0.

FRACTION NUMBER (5ml/fraction) m /e

Fig. 4.8. Chromatogram That Shows the Separation of Sodium Hippurate from Sodium Acetate and Acetic Acid by Fig. 4.9. Mass Spectra of Urinary and Reference Hippuric Gel Filtration Chromatography. Acid.

ORNL- DWG. 67-(2639A

b II SAMPLE 4.26 (a) HDO 7.93 (b) MARKER 8.10 (c) I STANDARD 4.30 (a) 7.97 (b) 8.10 (c)

II

I...... I.. .I. ..I... I ...I....I....I....I....I....I....I....I....I....1....I 9.0 0.0 7.0 6.0 5.0 4 .O 3.0 2.0 1.0 6

Fig. 4.10. Nuclear Magnetic Resonance Spectra of Urinary and Reference Hippuric Acid. 45

Likewise, uric acid was found to elute at 550 ml, as o-hydroxybenzoic acid (salicylic acid), a hydrolysis since the compound isolated from this fraction gave the product of aspirin. same MS (Fig. 4.11) and IR (Fig. 4.12) spectra as A paper on this work was presented and a reference uric acid. The identifications of both the paper was also published.2 * I hippuric and uric acid by this method confirmed the tentative identifications of these compounds described earlier. 23C. A. Burtis and K. S. Warren, “Identification of Urinary Constituents Isolated by Anion Exchange Chromatography,” A large unknown fraction eluting at 40 hr on the presented at the Symposium on Urinary Constituents of Low preparative system was concentrated and desalted and Molecular Weight, Oak Ridge National Laboratory, Oak Ridge, was successfully identified by MS and UV spectroscopy Tenn., Nov. 30-Dec. 1, 1967.

ORNL-DWG. 68-488 1 oc I I

MASS SPECTRA OF URIC ACID 75 i - e 0N\H 5c ?” F ,C=O - O&,NfiG\~~ W 0 z - z25 3 m :! a ! IS W roc I‘ I I I I I I I -> l- a MASS SPECTRA OF URINE FRACTION -1 w 75 Electron Energy - ctz 70 ev --__.-_-._ 20 ev 50 E -

25 k : -

I Ei I I1 I. ! I I: 0 I 50 70 90 I1 0 130 150 t70 190 210 230 M/e

Fig. 4.1 1. Mass Spectn of UMary and Reference Uric Acid. 46

ORNL-DWG. 68-12483 100

80 z m0 60 cn 2 a U + 40 + 2 W - ccV ------REFERENCE URIC ACID w 20- a URINARY SAMPLE -

0 4000 3600 3200 2800 2400 2000 1800 f600 1400 1200 1000 800 600 400 200 WAVE N U M BER , cm-’

Fig. 4.12. Infrared Spectra of Urinary and Reference Uric Acid.

4.3.b Anion-Exchange Chromatography of Table 4.6. Results of Anion-Exchange Chromatographf Hydrolyzed Urine of Acid- and Enzyme-Hydrolyzed Urine C. A. Burtis ~~ - Number of Peaks in Many compounds are excreted in urine as conjugates. Hydrolysis Hydrolyzed Urine The main conjugation reactions that occur in animals Lost Gained are those which involve glucuronic acid, sulfate, glycine, cysteine, methylation, and acetylation. To determine Acidb 22 7 whether any of the compounds associated with the p-GlucuronidaseC 9 7 Sulfatased 9 5 UV-absorbing peaks observed after anion-exchange Pepsine 9 8 chromatography of urine are conjugates, urine was p-Glucuronidase and 20 18 enzymatically and chemically hydrolyzed and the re- sulfatase mixturd sultant hydrolysate was chromatographed by anion- exchange chromatography. By comparison of urine uChromatogaphy was performed with a 0.45- by 200-cm chromatograms before and after acid or enzymatic stainless-steel column; 5- to 10-p Dowex 1-X8 resin; tempera- ture, 4OoC for 16 hr and 6OoC for 16 to 48 hr; operating hydrolysis, the presence or absence of urinary con- pressure, 1000 to 2000 psig; eluent, sodium acetate-acetic acid jugates can be determined. In the enzymatic hydrolyses, buffer at pH 4.4, varying in concentration from 0.015 to 6 M; a urine blank without the enzyme was carried through and average flow rate of eluent, 28 to 30 ml/hr. each incubation to determine the lability of the urinary bUrine of normal male adjusted to pH 1.0 with concentrated constituents to the incubation and hydrolysis condi- HCI and incubated at 75OC overnight. The pH was adjusted to tions. Table 4.6 gives the results of the various 4.4 before chromatography. hydrolyses. The data presented have been corrected for from normal male buffered to pH 4.7 with 0.1 M the gain or loss of chromatographic peaks due to the acetate and incubated for 48 hr at 37OC with 5000 Fishman units of Worthington Biochemical Corporation’s glucuronidase. reaction conditions. %rine from a woman in her eighth month of pregnancy was The acid hydrolysis resulted in the loss of 22 adjusted to pH 5.0 with 1 M acetate and incubated 72 hr at chromatographic peaks and the appearance of seven 37OC with 10 mg of sulfatase (Sigma Chemical Company’s new ones. It was also observed that the hippuric acid limpet type 11, 100 units). (benzoylglycine) peak was unaffected, which indicates eMale urine adjusted to pH 2.7 with 0.2 M citrate and that the amide bond contained in this type of conjuga- incubated 36 hr at 37OC with 10 mg of Worthington Biochemi- tion is resistant to the hydrolytic conditions. Condi- cal Corporation’s pepsin. tions known to hydrolyze this type of bond (6 M HCl, fUrine from a two-year-old girl, who has a neuroblastoma and has been treated with methylated purines, steroids, and radia- heat) were too harsh; chromatography of urine hydro- tion to the cranium was adjusted to pH 4.4 and incubated with lyzed under these conditions resulted in an 80 to 90% 300,000 Fishman units of bovine glucuronidase and 10 mg of loss of chromatographic peaks. limpet sulfatase for 72 hr at 37OC.

..._ ..... ~ 47

0 Enzymatic hydrolysis is milder and more specific than Studies of this nature are useful in ascertaining the acid hydrolysis. The conjugation of glucuronic acid with type of constituents contained in the column fractions the hydroxyl group of urinary constituents such as of urine that give the chromatographic peaks. If our ? steroids and aromatic acids is the type of conjugation assumptions are correct, then separatory procedures can most commonly found in urine. Hydrolysis of urine be devised to isolate a particular constituent for spectral with 0-glucuronidase resulted in the loss of nine and the analysis and identification. gain of seven chromatographic peaks. The section of the chromatogram between the elution volumes 325 and 4.3.c Fractionation of Urine by Gel 351 ml was definitely altered by 0-glucuronidase hy- and Anion-Exchange Chromatography drolysis (Fig. 4.13). In this example, two peaks are lost on glucuronidase hydrolysis. C: A. Burtis A second type of conjugation that involves steroids Prior investigation has indicated the feasibility of and aromatic acids is the conjugation of sulfate with the using gel chromatography to prefractionate raw aromatic hydroxyl groups of such compounds. Since urine.24 Separation of urine components by gel chro- the female hormones (estrogens) are steroids that matography on Sephadex G-10 yields as many as ten contain aromatic hydroxyls, the urine of a pregnant W-absorbing fractions (Fig. 4.14). The refractive-index female was hydrolyzed with sulfatase. This hydrolysis monitor indicates four peaks, three of which corre- resulted in the loss of nine and the gain of five spond to UV-absorbing fractions. The fraction that gave chromatographic peaks. To further investigate the the fourth peak was found to be strongly ninhydrin effect of glucuronidase and sulfatase hydrolyses on positive and to contain urea. urine, the urine from a two-year-old girl having a Because of incomplete resolution of four of the neuroblastoma was hydrolyzed with a mixture of the W-absorbing peaks, the contents of tubes from a two enzymes. The patient had been administered chromatographic run were pooled into six fractions. steroids for therapeutic reasons; therefore, a high The six fractions were concentrated and chromato- concentration of urinary steroids was expected. The graphed on a 1.25- by 200-cm anion-exchange column chromatography of the resultant hydrolysate resulted in packed with 20-E.(Dowex 1-X8. With this system, a a loss of 20 and a gain of 18 chromatographic peaks. typical chromatographic run requires 40 hr and resolves Preliminary investigation indicates that of the com- 70 to 80 chromatographic peaks. Figure 4.15 gives the panents corresponding to the peaks lost several are of a results obtained from the chromatography of these gel steroidal and several of an aromatic acid nature. fractions. The top chromatogram was obtained from * Urine was also hydrolyzed with the enzyme pepsin, a chromatography of 20 ml of whole urine; 83 chro- peptidase that cleaves amide bonds involving an are matographic peaks were resolved. The lower chromato- matic amino acid. Chromatography of this hydrolysate grams are those obtained by chromatography of the resulted in the loss of nine and the gain of eight respective gel fractions in which 18 peaks were observed chromatographic peaks. from fraction I, 30 from 11, 13 from III,63 from IV, 12 from V, and 17 from VI. Several of the peaks that were not well resolved in the chromatogram of a normal ORNL-WIG. 68-2141A NORMAL CONTROL GLUCURONIDASE urine were found in different gel fractions and appeared URINE URINE HYDROLYZED in their respective chromatograms as resolved peaks. URINE The increase in resolution is easily seen in Fig. 4.16 in 0.3 which a peak that was not resolved in the urine chromatogram appears as a single peak in the gel fraction. These results have confirmed that human urine is a complex biological fluid. The prefractionation of urine by gel chromatography followed by anion-exchange chromatography of the gel fractions has proven useful for increasing resolution and obtaining single peaks for ELUTION VOLUME (ml)

‘A 24C. A. Burtis, “Fractionation of Urine by Gel-Permeation Fig. 4.13. Anion-Exchange Chromatogram of Glucuronidase- Chromatography,” Anal. Chem Div. Ann. Progr. Rept. Oct. 31, Hydrolyzed Urine. 1967, ORNL-4196, p. 50. 48

ORNL- DWG. 68- 5866 RI 0.8 Chromatographic Conditions : Columns : 5.0 x 76crn+2.5 x 86cm Resln : G-IO , 40- 120p I IPI P 0.6 . mesh Eluent: dlstilled H20, 25OC Flow: 2.2 rnl /rnln EO . Sample: 5ml human 2: 0.4 a hair

0.2

O 200 400 600 800 4000 1200 1400 1600 1800 2000 2200

X W 0z W 2 I- V a (L LL W U

200 400 600 800 1000 1200 1400 1600 1800 2000 2200 ELUTION VOLUME, ml

Fig. 4.14. Chromatograms from the Fractionation of Human Urine by Gel Chromatography. , I, , *L

Q " @

P UJ

Fig, 4.15. Chromatograms from the Anion-Exchange Chromatography of Urine Prefractionated by Gel Chromatography. 50

separation of urine. A catalog of GC retention data27 ORNL-DWG. 68-214C has been compiled from the literature to aid in this 0.5 NORMAL URINE CHROMATOGRAM identification. The approach to the gas chromato- I graphic analysis of the urine fractions will involve desalting (Sect. 4.3.e), drying, and derivatizing the fraction prior to injecting it into the chromatograph. Fractions eluting from the GC will be collected for mass spectral analysis. 4.3.e Desalting of Fractions from the Anion-Exchange Chromatography of Urine W. C. Butts Initial studies indicate that derivatization which ren- ders the urinary constituents suitable for gas chro- matographic analysis cannot be performed in the presence of the large amount of sodium acetate present in the acetic acid-sodium acetate buffer used to elute the fractions from the anion-exchange column. Similar amounts of sodium chloride also interfere. With a nonpolar solvent such as hexane, solvent extraction of the aqueous fraction and of the residue left after lyophilization of the fraction gives negligible extraction of the acetate as well as of the urinary component. Polar solvents such as methanol extract both acetate and the urinary constituents. Aromatic and other ELUTION VOLUME UV-absorbing solvents are unsuitable, because UV monitoring is used as a method of detection. A Fig. 4.16. Increased Resolution of a Urine Anion-Exchange compromise solvent, isopropanol, gives the most suit- Chromatogram by Prefractionation by Gel Chromatography. able results. Lyophilization of the column fraction removes the spectral analysis. We are presently attempting to ana- acetic acid of the buffer and leaves the sodium acetate. lyze these resolved peaks by routine spectrometric Titration of the fraction with hydrochloric acid to analysis. convert the sodium acetate to acetic acid followed by A paper on this work was presented orally;2’ a lyophilization removes most of the acetate and leaves a manuscript was submitted for publication.2 residue of sodium chloride and the urinary compound. Most of the urinary compounds can be extracted into 4.3.d Gas Chromatographic Analysis of isopropanol from the sodium chloride residue. Refine- Fractions from the Anion-Exchange ments in this technique are being made. Chromatography of Urine Preliminary experiments indicate that ammonium W. C. Butts acetate can be removed by lyophilization without additional treatment. Further study may warrant the The recently acquired Micro Tek MT 220 gas chro- use of ammonium acetate in place of sodium acetate in matograph (GC) will be used to identify fractions the anion-exchange buffer. obtained from the anion-exchange chromatographic Several fractions desalted by the HCl titration- lyophilization technique have been submitted for mass spectral analysis. The spectra indicate that the samples 25C. A. Burtis, “Fractionation of Urine by Gel Filtration Chromatography,” presented at the 20th National Meeting, are contaminated and/or are mixtures and that addi- American Association of Clinical Chemists, Washington, D.C., tional separation (e.g., by GC) is necessary. Au~.18-23,1968. 26C. A. Burtis, “Fractionation of Human Urine by Gel 27W. C. Butts, Catalog of Gas Chromatographic Retention Chromatography,” submitted for publication to Clinica Chimica Data for Urinary Constituents and Related Compounds, Acta. ORNL-TM-2374 (May 13,1968). @- 51

4.3.f Gel Electrophoresis of Proteins 4.3.h Amino Acid Sequence of Mouse Hemoglobin A. L. Travaglini J. E. Attrill R. A. Popp3’ Study of polyacrylamide gel electrophoresis2 was The sequence in which amino acids exist in proteins is continued. Protein samples were separated in both basic of importance in studying biochemical evolution as well and acidic buffers. The effects of the presence and the biochemistry of Life. Each amino acid position in absence of stacking gels, incorporation of samples into as each protein can be considered to be a variable trait gels, and addition of samples in solution were studied. that has 20 potential levels of distinction. Because of In general, the sharpest separations seemed to occur the similarity of all mammalian hemoglobins, work has when the sample was added in a gel on top of a stacking been undertaken to study genetic factors in hemoglobin gel. Various stains were studied for detecting the with various strains of laboratory mice. The mouse was positions of the proteins; nigrosine seems to be the chosen, because it is easy to raise, grows rapidly, and is most sensitive. Procion Blue, a new dye, appears to have promise. It stains by reacting with the -NE- group in available in pure blood lines. Past has shown peptides; therefore, the intensity of the stain color is proportional to the concentration of protein. More ’Biology Division. study of the effects of buffers, such as citrate, borate, R. A. Popp, “The Separation and Amino Acid Composition phosphate, etc., on the separation of proteins is needed. of the Tryptic Peptides of the CY Chain of Hemoglobin from Many samples of papain-solubilized hamster tumor C57BL Mice,”J. BioL Chem 240, 2863 (1965). induced by adeno 31 virus were run for E. L. Candler, Jr.,29 and J. L. Jain~hill.~’The results were used by Table 4.7. Possible Amino-Acid Sequence of the p Chain them to locate the fraction of sample that contained T of C57BL Mouse Hemoglobin

~~ (or tumor) antigen. They then successfully isolated the Peptide Sequence tumor antigen. 12345678 4.34 Centriphoresis PT- 1 Val, His, Leu, Thr, Ala, GIu, Asp, Lys 9 10 11 12 13 14 15 16 17 A. L. Travaglini PT-2 Ser, Ala, Val, Gly, Ala, Leu, Tyr, Gly, LYS 18 The initial work with centriphoresis was described BT-3 Val,Asn, Ala, Asp, Glu, Val, Gly, G~Y,Gh, Ala, Leu, ear lie^.^' Every serum protein sample tried has been G~Y,A rg separated into three or four fractions, usually four, PT4 Leu, Leu, Val, Val, Tyr, Pro, Tyr, Thr, Glu, Arg when centriphoresed. Albumen has been identified as 0-5 Tyr, Phe, Ser, Ser, Phe, Gly, Asp, Leu, Ser, Ser, Ala, part of the fastest-moving fraction and globulins as part Asp, Ala, Ile, Met, Gly, Asn, Ala, Lys of the slowest-moving fraction. Components of the other fractions have not yet been identified. Cen- PT-6 Val, Lys triphoresis appears to be a convenient way to separate BT-7 Ala, His, Gly, Lys albumen from globulins in serum samples. fl-8 LY S Before more studies with new buffers are done, a new rotor is needed that has provision for cooling the rotor pr-9 Val, Ile, Thr, Ala, Phe, Sei, Asp, Gly, Leu, Asn, His, Leu, Asp, Ans, Leu, Lys and its contents and a greatly enlarged compartment for the electrode, buffer, and sample. Heating of the sample pr-10 Gly, Ser, Phe, Ala, Thr, Leu, Ser, Glu, Leu, His, Cys, and the resulting increase in diffusion has been the only ASP, LYS problem encountered during use of this method. pr-11 Leu, His, Val, Asp, Pro, Glu, Asn, Phe, Arg BT-12 Leu, Leu, Gly, Asn, Val, Leu, Val, Ile, Gly, Leu, Met, ”A. L. Travaglini, “Electrophoresis of Proteins,” Anal His, His, Ile, Gly, Lys Chem Div. Ann Prop. Rept. Oct. 31, 1967, ORNL-4196, p. 51. fl-13 Asp, Phe, Thr, Pro, Ala, Ala, Gly, Ala, Ala, Phe, Glu, LYS Molecular Anatomy~- Program. 140 141 142 143 30Loanee to the Molecular Anatomy Program; Staff Asso- m-14 Val, Val, Ala, Gly, Val, Ala, Ala, Ala, Leu, Ala, His, ciate, U.S. Public Health Service-National Institutes of Health. 144 LYS 31N. G. Anderson, A. L. Travaglini, L. C. Patrick, R. L. 145 146 Jolley, and E. C. Candler, Jr., “Centriphoresis,” AnaL Chem pr-15 Tyr, HIS Div. Ann Prop. Rept. Oct. 31, 1967, ORNL-4196, p. 52. 52 the complete sequence of amino acids in the a chain of chromatography. These two forms showed that when G the hemoglobin of C57 Black, a common pure-bred valine occurs in position 62, only asparagine is found in strain of laboratory mouse. We are still working on the position 68 and that when isoleucine occupies position sequence of the 0-chain hemoglobin of this same type 62, only serine is present at position 68. Analytical of mouse; Table 4.7 shows a proposed sequence. The results also indicated that the position 62Va1-68ASn portions in italics indicate a proven sequence. form is 30% and the 6211e-6SSer form is 70% of the Procedures for sequencing these chains have been total aT9 peptide. given already.15 The changes that have been made to The finding of two forms of aT9 in the same ratios as improve the procedures include using a longer pH the two forms of aT4 supports the theory that the gradient for separating the peptides (obtained by amino acid duplexity at these three positions results enzymatically splitting the chain) on a Dowex 50-X2 from gene duplication rather than from translational cation-exchange chromatographic column only. Pre- ambiguity. viously, this had been done by means of a run through first a cation- and then an anion-exchange column. 4.4 ASSISTANCE TO OTHERS Also, improvements in the paper chromatographic J. E. Attrill separations of both peptides and individual amino acids in micromolar concentrations have been made by K. M. Assistance has frequently been rendered to other groups in the Laboratory. For E. S. Rogers of the Work with the a chain of another strain (C3H) of Biology Division, samples of protein from papillomas laboratory mouse was completed; an article on this found on two varieties of rabbits were hydrolyzed and work will be published. checked for amino acid content. These proteins con- tained the enzyme arginase. It was intended to show 4.3.i Amino Acid Substitutions that these papillomas contained different types of arginase and to pinpoint these differences. Present J. E. Attrill K. M. results are still inconclusive because of the small R. A. Popp3 W. S. McErwin3 amounts of samples available. Laboratory and technical assistance has also been A paper is being published35 which gives evidence given to R. H. Stevens of the ORGDP Instruments and that gene duplication rather than translational varia- Controls Systems Development Department while a tions is probably the basis for amino acid ambiguity in micro amino acid analyzer was being designed and built. the a chain of mouse hemoglobin. The a chain of the Moderate success has been achieved on this program. A hemoglobin of the C3H type laboratory mouse has small high-temperature high-pressure reaction bath, three positions that contain alternate forms of amino which reduces ninhydrin reaction time from 15 to -2 acids. Position number 25 of the chain may be glycine min, has been built and tested. or valine, position 62 is isoleucine or valine, and Also, I. B. Rubin of this Division was assisted in position 68 may be serine or asparagine. The chro- procuring and analyzing standards that have been used matographic characteristics of the tryptic-peptide- to develop a new ultrasensitive method for the determi- digestion fragments are altered depending on which nation of amino acids (Sect. 4.1.1). amino acid is in each of these positions. Analysis of the Several types of paper and thin-layer chromatographic two chromatographically separable forms of the tryptic (TLC) procedures have been tested for possible use in peptide aT4, which include position 25 in the chain, determining phenylthiohydantoin derivatives of amino indicates that 70% of this peptide contains valine and acids. This is the form in which amino acids will be 3% contains glycine. Tryptic peptide aT9, when removed sequentially from a protein by an automatic recovered, contained positions 62 and 68 in the a chain. sequenator that is being built in connection with the Two forms of the peptide were also separated by paper Molecular Anatomy Program. Attempts to reproduce published in which concentrations of these compounds are determined rapidly by TLC have not 34Research Fellow in the Biology Division; from the Max- Planck Institute for Biochemistry, Munich, Germany. been entirely successful. 35 K. M. Hike and R. A. Popp, “Gene Duplication as the Basis for Amino Acid Ambiguity in the (%Chain Polypeptides of 36J. 0. Jeppsson and J. Sjoquist, “Thin-Layer Chroma- n- Mouse Hemoglobins,” accepted for publication in the Pre tography of PTH Amino Acids,” Anal Biochem 18,264 ceedings of the National Academy of Sciences. ( 1 96 7). / 53

X-Ray and Optical Spectrochemistry

Cyrus Feldman

5.1 X-RAY SPECTROSCOPY freedom (the vertical slope of the totally reflecting mirror) and can still accommodate replaceable partially H. DUM W. transparent mirrors. Inconel-coated mirrors have been Development work is in progress on a computer code found to be superior to rhodium-coated mirrors with for determining crystal lattice spacings and parameters regard to achromaticity of the reflectance/trans- directly from film or stripchart measurements. It is mittance ratio. necessary at present to supply Miller indices to obtain The optimum conditions for use of the beam splitter the appropriate lattice parameters, but it should be depend on the type of spectrograph with which it is possible to eliminate this inconvenience. used (Table 5.1). If the stigmatic position of the Electron-probe studies of high-phosphorus (-10 wt % spectrograph is not at the slit, the height of the light P) organic compounds have shown that sulfur at the source and the height of the opening in the Hartmann 0.1-wt % level can be detected with 95% confidence in diaphragm must be limited to the degree necessary to such compounds. The limit of detection is now gov- prevent vignetting in or beyond the beam splitter. erned by the inhomogeneity of the sample (chemical and/or physical) rather than by the ratio of peak to 5.3 CHEMICAL PRECONCENTRATION OF background counting rates. TRACE ELEMENTS IN BONE ASH Cyrus Feldman F. S. Jones 5.2 BEAM SPLITTER FOR USE IN CALIBRATING SPECTROGRAPHIC EMULSIONS 5.3.a Reagent Purification Cyrus Feldman The formic, acetic, and especially the tannic acid used in the modified Mitchell-Scott procedure’ are potential On the basis of previous experience,’ a beam splitter sources of trace-element contamination and must be support was constructed that has only one degree of

‘C. Feldman,. “Beam Splitter for Use in Emulsion Cali- ’C. Feldman and F. S. Jones, “Spectrographic Analysis of bration,” Anal Chem Div. Ann Bop. Rept. Oct. 31, 1967, Tissue Ash,”Anal Chem Div. Ann Prop. Rept. Oct. 31, 1967, ORNL-4196, p. 55. ORNL-4196, p. 56.

Table 5.1. Optimum Conditions for Use of Beam Splitter with Fully Stigmatic and PartiaUy Stigmatic Spectrographs

Optimum Setting for Condition Fully Stigmati@ Spectrographs Partially Stigmaticb Spectrographs

Location of beam splitter Adjacent to slit Adjacent to slit Location of image-forming Iens Immediately in front of beam splitter At stigmatic position of spectrographC Location of Hartmann diaphragm At or close to slit At stigmatic position of spectrographC Maximum height of opening in Half the distance between the centers About 2 mm; limit set by onset of Hartmann diaphragm of the emergent beams vignetting Location of image of light source First internal optical element of First internal optical element of spectrograph (collimator or grating> spectrograph (collimator or grating)

~~ aAll prism spectrographs; the Ebert and Wadsworth (Jarrell-Ash Corp.) and Quantograph (Applied Research Lab., Inc.) grating mountings. bThe Eagle (Baird-Atomic, Inc.) and Abney (Applied Research Lab., Inc.) grating mounting. %pecified by manufacturer. 54

A purified before use. A preliminary precipitation with Table 5.3. Composition of Complete Process 8-hydroxyquinoline at pH 4.0, followed by extraction, Blank for Collection of Trace Impurities from was effective for removal of copper but would be either Bone Ash (3-g Sample) by a Modified Mitchell-Scott Procedure less successful or impractical for the removal of other contaminants. Use of a mixed-bed ion-exchange column Amount Presenp Impurity (hydrogen-form Dowex 50W-X8 and chloride-form (pg per gram of bone ash) Dowex 1-X8) was the most generally effective of the procedures tested. Table 5.2 gives the results of the Ag 0.07 Ca 0.07 application of these two procedures to the purification cr 1.1 of tannic acid. cu 0.1 The purified material was analyzed spectrographically Fe 4 by a lithium carbonate matrix-dc arc procedure. Since Mg 0.4 only 0.2 g of tannic acid is used in the Mitchell-Scott Mo 0.4 Na 14 procedure, the quantity in micrograms of each impurity Ni 0.9 contributed by this reagent would be one-fifth the Pb 0.1 amount shown in Table 5.2. Similar results were Si 15 obtained for other reagents used in the procedure. Ti 0.1 Zn 4 The analysis of a total-process blank, which included Zr 0.03 all reagents and all manipulations, gave the results shown in Table 5.3. In future development work, the recovery of trace ‘The following elements were not detected, with the indi- elements added to the original bone ash will be cated limits of detection (pg/g): measured. 0.001 to 0.01 Ba, Be, Er, Eu, Ge, Lu, Sc, SI, V, Y, Yb 0.01 to 0.1 Au, Bi, Co, Dy, G,a, Gd, Hf, Ho, In, Nb, Nd, Pd, PI, Pt, Rh, Ru, Sm, Sn, Tb, Th, Tm ’ 0.1 to 1 As, Cd, Ce, 11, Re, Ta, Te, U, W Table 5.2. Impurities Remaining in Tannic Acid After Its Purification by the Mixed-Bed Ion-Exchange and the 8-Hydroxyquinoline Extraction Procedures

Concentration (pgglg) 5.3.b Removal of Phosphate Impurity After Mixed-Bed After 8-Hydroxyquinoline Ion Exchange Extraction Tests showed that a two-compartment electrodialysis cell that contains an Ionac MA-3475XL anion-per- Ag 0.005 0.005 meable membrane is more efficient than a three-corn- A1 0.5 5.2 partment cell in removing phosphate from a sample B 0.3 1.6 solution. High currents give fast phosphate removal, but Ba <0.004 0.05 Ca 1.6 160 resistance heating of the solution limits the current Cr 0.2 0.3 permissible. Since the use of such a cell involves the cu 0.3 0.3 possibility of losing trace elements by deposition on the Fe 0.3 0.2 cathode (Pt wire), a way was sought to strip the 120 K 10 cathode. Chemical stripping is effective only when aqua Mg 0.2 16 Mn 0.02 0.2 regia is used; and the use of this agent inevitably adds Mo <0.03 0.03 platinum to the sample. Graphite cathodes are satis- Na 20 52 factory and can be wet-ashed to give complete recovery Ni 0.04 0.04 of trace elements. However, the wet-ashing is slow and P <6 12 considerably increases the danger of accidental contami- Pb 0.04 0.26 nation. Rhodium metal is more satisfactory than either FY 0.08 c0.08 Sn <0.04 0.26 platinum or graphite, since it functions well as a SI 0.02 0.12 cathode and is not affected by the aqua regia stripping Ti 0.1 0.2 process. Tracer tests showed that at least 94% of the V

Q 5.3.c Possible Loss of Cesium During Ashing of Bone h02,cadmium in concentrations as small as 0.1 pg/g can be measured routinely. To check on the possible loss of cesium during the ashing of bone at 45OoC, a sample of bone meal was 5.4.c Determination of Traces of Bismuth treated with 137Csin dilute H3P04 solution and was in LiF-BeF2 Mixtures ashed. The ash was dissolved in nitric acid. Essentially Likewise of interest is the extent of contamination of all the Cs was recovered. molten LiF-BeF2 by bismuth during the molten- bismuth extraction of the rare-earth elements. To 5.4 MISCELLANEOUS TRACE DETERMINATIONS determine the trace amounts of bismuth, the LiF-BeF2 INVOLVING CHEMICAL PRECONCENTRATION sample is dissolved in perchloric acid, and fluoride is Cyrus Feldman N. Marion Ferguson eliminated by evaporating the solution to fumes. The residue is dissolved, and the solution is treated with 10 5.4.a Determination of Traces of mg of iron as ferric chloride and brought to pH 4.5. RareEarth Elements in Bismuth Tracer experiments with 207Bishow that the resulting (Carrier-Free Procedure) ferric hydroxide precipitate carried bismuth quanti- In the reprocessing of used MSR fuel by molten- tatively. The precipitate is then redissolved in 6 N HC1. bismuth extraction, it is essential to know the degree to The iron is extracted with methyl isobutyl ketone, and which fission-product rare-earth elements are extracted the bismuth in the residual solution is determined by into the bismuth. A method was therefore developed atomic absorption spectrometry. The conveniently at- for determining the rare-earth elements in bismuth at tainable absolute limit of measurement is 0.5 pg of Bi; the ppm concentration level. The bismuth sample is for the 20-g samples analyzed, this limit corresponds to dissolved in -2 M HN03, and the pH of the solution is 0.025 g of Bi per gram of LiF-BeF2. adjusted to 1.0 with ”,,OH. The solution is then warmed. Quantitative precipitation of coarse-grained 5.5 DETERMINATION OF SILICON IN Bi02(OH)N03 results. The precipitate is centrifuged CURIUM OXIDE (244Cm203) off and dissolved in 2 M HN03, and the precipitation is Anna M. Yoakum Cyrus Feldman repeated. The supernatant solutions are combined. Tracer studies show that rare-earth elements remain 5.5.a Previous Status of Problem quantitatively in the supernatant solution. These ele- Many trace elements, including silicon, can be deter- ments can then be determined by flame photometry or mined in curium oxide by the carrier distillation- emission spectroscopy. spectrographx procedure with a reproducibility factor of-2.’ It is difficult to estimate the accuracy of this 5.4.b Determination of Cadmium in Plutonium method, since meaningful chemical checks are often To ensure that nuclear-grade plutonium meets speci- impossible, especially in the case of silicon. Additional fications, cadmium must be determined in PuOz at the uncertainty is introduced by the fact that the lack of 0- to I-pg/g level. The procedure consists in fusing the spectrographically pure curium oxide forces the use of PuOz with ammonium bi~ulfate,~94 removing the plu- other materials (e.g., neptunium oxide) as the principal tonium from solution by anion exchange, treating the component of standards. Since almost any substantial cadmium-containing eluate with ammonium pyrrolidine difference in chemical or physical properties among dithiocarbamate at pH 4.5, and extracting the resulting samples (e.g., particle size, thermal history, homoge- cadmium complex into methyl isobutyl ketone. The neity) can introduce bias into this type of analysis: it organic phase is evaporated, wet-ashed, and analyzed by appeared desirable to develop a method independent of atomic absorption spectrometry. In I-g samples of carrier distillation for determining silicon in curium oxide.

3C. Feldman, “Ammonium Bisulfate Fusion. Application to ’“Curium Oxide: Trace Impurities, Spectrochemical, Carrier Trace Analysis by Spectrochemical and Other Techniques,” Distillation Method,” Savannah River Plant Laboratory Manual Anul. Chem 32,1727 (1960). Code: Imp/Curium Oxidel, March 17,1967. 4G. W. C. Milner, A. J. Wood, G. Weldrick, and G. Phillips, 6M. Buffereau, G. Crehange, S. Deniaud, and C. Leclainche, “The Determination of Plutonium in Refractory Materials by Spectrochemical Analysis of Impurities in Plutonium and Its Electrometric Methods After Dissolution by Fusion with Am- Compounds (in French), Commissariat a I’Energie Atomique, -A monium Hydrogen Sulphate,” Analyst 92, 239 (1967). Saclay, France, CEA-R-305 1 (January 1967). 56

5.5.b New Method ORNL-DWG. 67-1368 100 I I I I The approach decided on was to dissolve the curium 0 244cn-l oxide in acid, remove curium and ionic impurities by -1 152~"-154~" J . electrodialysis through cation- and anion-permeable W V membranes, evaporate the residual solution or suspen- [L w sion to dryness, and spectrographically determine the I- z silicon in the residue (dc arc, Li2C03 matrix, argon- W oxygen atmosphere). A three-compartment Lucite cell 1c was built that has an Ionac MC-3470XL cation- z (3 permeable membrane, which separates the center z z (sample) compartment from the cathode compartment, a and an Ionac MA-3 148 anion-permeable membrane, 5 which separates the sample compartment from the [L >- anode compartment. The capacity of each chamber is c_ 21 -125 ml. To check the efficiency of the cell for t- V removing the elements from the sample compartment, a -1 tests were then made with tracer 244Cm and ls2Eu- U z Eu and with stable lithium. The tests showed that (3 [L only 0.1% of either the 244Cm or the 1s2E~-'s4E~0 originally placed in the sample compartment remained LL 0 after 4.5 hr of electrodialysis at 2 A; Fig. 5.1 gives the 8 0.t rates of removal. Flame photometric tests showed that the l-pg/ml concentration of lithium originally present I I I I ! 2 3 4 5 6 had been reduced to <0.0002 pg/ml. Thus, the proce- TIME, hr dure seems to be effective for cations of various weights and structures. Fig. 5.1. Rates of Removal of 244Cm and 1s2Eu-154E~ from 1 N "03 by Electrodialysis Through Permselective 5.5.c Recovery of Silicon Membranes. This method is based on the assumption that, regardless of their initial chemical states, all the silicon atoms originally present remain in the sample compart- ment, that is to say that any silicate radicals (SiO,") the cell was not kept covered during electrodialysis, the present are converted to colloidal particles of hydrated absolute blank per exposure was 7.2 pg of Si. When the , which, like the mineral forms of silicon, cell was kept covered, the blank was 1.5 f 0.1 pg of Si. are incapable of penetrating either membrane. Recovery Thus, for the analysis of a 100-mg sample, the Si blank tests were therefore run on silicon introduced both as would be 1.5 pg. It is estimated that, if the absolute sodium silicate (40 pg of Si) and as powdered quartz blank is reproducible to within kO.1 pg, 0.3 to 0.5 pg of (45 pg of Si). Recoveries were 101 f 8% and 101 ? 6%, Si can be detected in a 100-mg sample at the 95% respectively. confidence level. The relative standard deviation of measurements of total Si is 5 to 10%. 5.5.d Blanks 5.5.e Radioactive Contaminants In a combined chemical enrichment-spectrographic procedure, the useful limit of concentrational sensi- Any constituent of the sample that, like silica, forms tivity is determined by the weight of sample repre- particles of colloidal size or larger under the experi- sented in a single spectrographic exposure and by the mental conditions or is present as an undissolved total blank per exposure (from chemical treatment, particle will accompany the silica to the spectrographic atmospheric dust, electrode impurities). Test electro- electrode. If this constitutent is radioactive, suitable dialysis runs made in a conventional fume hood (linear safety precautions must be taken while making the velocity of air at face -125 ftlmin) showed that when spectrographic exposures. / 57

Mass Spectrometry

A. E. Cameron

6.1 SPARK-SOURCE MASS SPECTROMETRY has been in constant service during the past year. A wide variety of compounds has been run, both to J. R. Sites J. A. Carter collect reference spectra and to aid in the identification The solution spark-source technique described pre- or elucidation of structure. Truxenes, which are poly- viously’ was used to make a trace characterization nuclear aromatic hydrocarbons, were investigated for analysis of 242Pu(fl12 = 3.79 X lo5 y). The sample the Y-12 Plant with useful results. The spectra of electrodes were prepared for spark-source analysis in methyl and butyl phosphates were taken for the the Transuranium Research Laboratory by drying 5.5 Chemical Technology Division. Some fluorinated alkyl pg of 242Pu, which had been spiked with , on phosphates are currently being scanned; attempt is two gold electrodes. Twenty-one general-element con- being made to verify the positions of the fluorine atoms taminants in the range 0.001 to 0.6 wt % were found. in an incompletely fluorinated tripentyl phosphate. In addition, transuranium isotopes of masses 240 These samples were submitted from a university, as (0.013 wt %) and 244 (0.009 wt %) were also present. were some organometallic compounds. Products from A set of 30 samples of ashed leaves from many the radiation-induced oxidation of cyclohexane were different plants were analyzed to determine the distri- examined. bution of the rare-earth elements in the leaves. A few Most of the work has been related to the Body Fluids milligrams of each sample was mixed with an equal Analyses Program (Sect. 4.3). Spectra have been re- weight of pure bismuth powder, and the mixture was corded of about 20 steroids and steroid conjugates and pressed isostatically as enriched ends on bismuth- of some 50 other compounds that are known to be powder rods. The same was done for a set of 25 samples constituents of urine. Efforts to identify compounds of ashed wood. collected from the high-pressure chromatographic The trace elements in several samples of CsGd(HFA)4 columns were not entirely successful because of the were determined (HFA = hexafluoroacetylacetonate). small sizes of the samples, presence of impurities, and This compound is unusual in that it is a stable volatile difficulty of removing the buffer salt. compound of rare-earth elements. Although the low-resolution mass spectrometer was Many samples of materials used to make target foils designed to be attached to a gas chromatograph, the for cyclotron bombardment were analyzed for trace- only gas chromatographic samples that have been run element contaminants. These materials included the were trapped as they emerged from a column not metallic forms of the following isotopically enriched connected to the spectrometer. It now appears desirable elements: 24Mg,48Ca, 50Ti, 90Zr, 142Nd, lS6Gd, to connect the two instruments. * Er, and Pt. Metallic and were ’ 6.3 SURFACE IONIZATION also analyzed. STUDIES For the Argonne National Laboratory, the following G. R. Hertel materials were analyzed for trace elements: a set of (Sc 6.3.a Surface Ionization of UF4 at Various Gd) samples, UB2, UC, US2, Cu-Mg, Zr02, Sc, Ho, + Oxygen Pressures and Er. The high-neutron-cross-section contaminants in T-1 1 1 Studies of the emission of uranium and uranium alloy (Ta-W-Hf) were analyzed for boron, cadmium, and oxide ions from hot tungsten ribbons233 have been the rare-earth elements. ‘J. R. Sites and J. A. Carter, “Spark-Source Mass Spectrometry,” AnaL Chein Diu. Ann Rept. Oct. 31, 6.2 LOW-RESOLUTION MASS SPECTROMETRY Progr. 1967, ORNL-4196, p. 59. OF ORGANIC COMPOUNDS 2G. R. Hertel, “Surface Ionization. I. Desorption of U+ Ions W. T. Rainey from W and Re Surfaces,” J. Chem. Phys. 47,133 (1967). 3G. R. Hertel, “Effect of Oxygen Contamination on the The low-resolution mass spectrometer, which was Surface Ionization of Uranium Tetrafluoride,” Anal. Chem Div. built for general-purpose scanning of organic spectra, Ann. Progr. Rept. Oct. 31, 1966, ORNL-4039, p. 48. 58

continued and extended; the results are interesting. The cated mixture or series of surface reactions. Further temperature dependence of the ion emission intensities study is required. (I's) and of the mean residence times (7's) of the ions on the tungsten have been studied at oxygen pressures 6.3.b Ionization-Potential Measurements of 1 X 5 X 1 X and 3 X torr. At G. R. Hertel D. H. Smith a filament temperature of -2500"K, U+ emission de- creased rapidly as the oxygen pressure was increased. The surface-ionization comparison technique4 is The UO' and UO,' emissions reached maxima at being used to evaluate the first ionization potential of greater intensities and at higher temperatures than they the actinide elements. A tentative value of 7.5 f 0.3 eV did prior to the introduction of oxygen. In addition, a has been determined for thorium. second UO,' maximum with an intensity an order of magnitude greater than the first was observed at a lower temperature. Table 6.1 summarizes these data. 6.4 MASS SPECTROMETRIC DATA REDUCTION A study of 7 with respect to temperature indicates the W.H. Christie H. S. McKown possibility of three distinct evaporation processes. The U' ion evaporation occurs at high temperatures with an In June an IBM 1130 computer was delivered and evaporation energy (Ei)of 7.50 f 0.09 eV.' ,3 installed. The intention is to have this hard wired to At temperatures below -1470°K, the log (1/~)vs 1/T several mass spectrometers to provide immediate calcu- plot of the data again approximates a straight line and lation of the data, which are presently recorded on thus indicates a dominant evaporation process with a punched paper tape and calculated by the computing characteristic energy. A least-squares fit of the data in center at ORNL or ORGDP. Work is under way on the this temperature region gave Ei = 6.9 f 0.4 eV. At these interfacing that is necessary to permit the multichannel

temperatures, UO, + is the only ion detected and thus analyzers to dump data direct to the computer. The one may consider this Ei of 6.9 eV to be the Ei of high-resolution mass spectrometer will be connected in U02+ from a tungsten surface. a way such as to accumulate data directly in the IBM The log 1/7 vs 1/T relationship has one other segment 1130, since the storage in a 400-channel analyzer will that approximates linearity. This segment is between be inadequate. The device has been programmed to -1750 and -2250°K. At an oxygen pressure of 5 X handle most of the computational requirements of the torr, the Ei deduced from this region is 1.6 f 0.1 digital recording instruments. Thus far, the operation eV. The UOz+ emission dominates in this temperature has been very successful. region when the atmosphere is oxygen, but no clear-cut assignment of this energy to any simple process can be made. 4G. R. Hertel, "Ionization Potential Measurements by Surface The behavior of the 7's and the I's in the mid- Ionization," Anal. Chem Div. Ann Progr. Rept. Oct. 31, 1966, temperature region implies the existence of a compli- ORNL-4039, p. 49.

Table 6.1. Temperatures and Relative Intensities (Z) of Oxide Ion Maxima uo; uo+ 02 Pressure 1st Maximum 2d Maximum Temperature (ton) Z Temperature Temperature (OK) I Z (OK) (OK)

1 x 2375 1.0= 1830 2.4 1435 3.8 5 x lo-* 2500 1.5 1860 3.0 1490 -2 8 1 x 2565 1.8 1900 3.6 1505 -26 3 x 2625 2.3 1945 3.9 1525 -24

aAll intensities normalized to this point. 7. Optical and Electron Microscopy

T. E. Willmarth T. G. Harmon H. W. Wright

7.1 RESEARCH ASSISTANCE IN ELECTRON 80°C. It was learned that the lanthanide hydroxides MICROSCOPY AND ELECTRON DIFFRACTION differ greatly among themselves in the time necessary to change from an amorphous to a well-ordered state. Electron microscopy and electron diffraction have Some crystallize after minutes, whereas others are still been used in a wide variety of fundamental and applied undergoing changes toward crystallinity after months of research to study materials of interest in nuclear aging. Figure 7.1 shows that cerium hydroxide is almost technology and in other scientific disciplines at OhVL completely crystallized after 70-min aging at 25°C. and Y-12. Figure 7.2 shows that after 99.7-day aging, ytterbium hydroxide appears to have changed from the amor- 7.1 .a Lanthanide Hydroxide Sols phous state but is only weakly crystalline. The relative With both electron microscopy and electron diffrac- crystallinity of the two materials was checked by tion, the hydroxide sols of the following lanthanide electron diffraction. It appears that the lanthanide elements were studied: Ce, Dy, Gd, Ho, La, Lu, Sm, Tb, hydroxide sols can be classified into tight subgroups Tm, Yb, and Y. The metamorphosis to the crystalline strictly on the basis of aging characteristics. The effect stage was observed either as the material aged at 2S0C of dilution and pH on the aging characteristics of or as it aged at 80°C after it had been heated initially to certain lanthanide hydroxide sols was also studied.

-0.33~ -0.33fi

Fig. 7.1. Electron Micrograph of Cerium Hydroxide Aged 70 Fig. 7.2. Electron Micrograph of Ytterbium Hydroxide Aged Minutes. 99.1 Days. 60

7.1.b Studies of Absolute Filters was used to determine what Varcum specifications are required to produce a good sponge. Large drops of the An engineering group is studying the deterioration of material, which was suspected to contain solids, were absolute filters that occur when they are subjected to diluted with furfuryl alcohol, the solution was broken high temperatures. In cooperation with that group, up in an ultrasonic generator and then diluted further changes in the filter structures were observed under the with furfuryl alcohol. The solids were collected by Philips EM 200 electron microscope at the extremely centrifugation, and the remaining furfuryl alcohol was low magnification possible with it. Thin layers of filter material were stripped from the test samples by means decanted. The solids were then redispersed in ethyl of cellulose acetate tape and were sandwiched in alcohol, and portions of the dispersion were deposited “hinged” 50- to 100-mesh copper grids for electron on carbon-substrated 200-mesh copper grids for elec- microscopy. Figure 7.3 shows a section of the absolute tron microscopy. Figure 7.5 shows the rosette appear- fdter before it was heated; Fig. 7.4 was taken after the ance of typical particulates common to both “good” and “bad” Varcum. Figure 7.6 shows the chains of filter was heated for 15 min at 400°C. The electron spherical resinous particles found in “bad” but not in micrographs indicate that the physical breakdown of “good” Varcum. the filters is caused by burnup of the binder material followed by melting of* the glass fibers of smallest 7.1.d Other Research Assistance dianeter. 7.l.c Studies of Varcum Electron diffraction (both optical and electron) and microscopy were used to study many other materials of Varcum is a viscous derivative of furfuryl alcohol used research interest. Among these were colloids in molten to fabricate carbon-fiber sponge. Electron microscopy salts; oxide sols of zirconium, hafnium, , and

PEM-200- 8768

U U 5.0~ 5.0~

Fig. 7.3. Electron Micrograph of Absolute Filter Before It Fig. 7.4. Electron Micropaph of Absolute Filter After It Was Was Heated. (Binder still present.) Heated 15 Minutes at 400 C. (Binder has disappeared.)

. 61

PFM -200-9325

U 1.Op

Fig. 7.6. Electron Micrograph of Resinous Chains Found in -1.op “Bad” But Not in “Good” Varcum.

Fig. 7.5. Electron Micrograph of Typical Particulates Found in Both “Good” and “Bad” Varcum. strated. We suggested the method of collecting the particles, which proved to be satisfactory. uranium; nitrides of uranium and boron; the oxidation products from Hastelloy N heated to 1800°F in air; 7.3 INSTRUMENTATION tantalum oxide; uranium oxide-tungsten oxide pow- ders; industrial graphite; natural carbon; and vaporized An electron-beam device for the vacuum vaporization sodium chloride. of metals and oxides has been installed to produce high-purity fims for study and for use as substrates and 7.2 ELECTRON MICROSCOPY OF in shadow-casting. A Philips 100 B electron microscope RADIOACTIVE MATERIALS will be moved to Building 3019 to replace the Philips 100 A microscope used for the examination of radio- Conjointly with the Health Physics Division, we active materials. The Philips EM 300 electron micro- examined particles of 238Pu02in relation to NASA scope is being installed in the Transuranium Processing space experiments. Plant. The purchase of a scanning electron microscope The presence of radioactive particulates in the vapor ’ to meet a growing demand for such service has been phase over the molten salts in the MSR was demon; requested. 62

8. Nuclear and Radiochemistry

W. S. Lyon H. H. Ross

8.1 ACTIVATION ANALYSIS laboratory hood; it is carried to and from the irradia- tion chamber through the plumbing of the pneumatic 8.1 .a Air-Floating Sphere for Homogeneous transfer system; and, during bombardment, the same Photon and Neutron Irradiation in Remote plumbing provides the supporting air cushion that also Facilities of Uneven Flux cools the sphere while imparting the double-axis motion Enzo Ricci T. H. Handley M. G.Willey’ to it. The metallic sphere does not suffer significant radiation damage. One extra advantage of the sphere is Activation analysis and other nuclear techniques that, because of its shape, it can run more easily than normally require comparative bombardment of two or the usual cylindrical rabbits through the pipes of the more samples. For this purpose, irradiation in a transfer system, thus allowing for sharper bends in the homogeneous flux is mandatory. However, photon and pipes and diminishing the danger of clogging. neutron fields provided by conventional electron accel- The development of this system will continue. erators and neutron generators are uneven. To remedy this situation, a simple device was conceived and was 8.1 .b Photon and Fast-Neutron Activation tested in its preliminary stage. The device consists of an Analysis at The Oak Ridge Electron Linear aluminum sphere that contains four sample capsules. Accelerator (ORELA) The sphere can be transferred pneumatically to the Enzo Ricci M. G. Willey’ bombardment chamber, where it is suspended in an upward stream of air which also causes it to spin around Progress has been made in the design of the pneu- a precessing axis. Even if these rotations are not matic rabbit facility for activation analysis to be performed perfectly, the movement of the floating installed at the ORELA (Building 6010). The prelimi- sphere is still sufficiently random to guarantee homo- nary plans for this facility4 have been changed slightly. geneous flux. Tests were run in a 14-MeV neutron flux; The tantalum target designed for physics experiments four fluorine samples were activated for only 1 min by will also be used to produce photons and fast neutrons the reaction F(n, 2n)’ F, 1 10 min. The S of the F for activation analysis. A movable irradiation assembly count rates of the samples was only 0.83%. has been designed that can be positioned at the back of This device is unique in its simplicity of operation; the tantalum target for activation experiments. This the simple air-floating sphere replaces complicated same assembly will be used for irradiation with both mechanical equipment. The best previous systems con- photons and fast neutrons. When activation experi- sist of a pneumatic carrier and a dual-axis ments are finished, the assembly will be withdrawn to Two requirements are inherent to their design: (1) prevent disturbance to physics work. The sample transmission of movement to the rotator and (2) capsules will be located inside an aluminum ball (Sect. alignment of pneumatic pipes with the rotator after 8.1 .a), which will travel through the piping to the each irradiation to ensure safe retrieval of samples. Our irradiation site. After bombardment, the ball will be system has none of these difficulties, because the sphere received in a lead enclosure, where it will be opened by itself is the rotator. It is loaded and unloaded in a remote manipulation to release the sample capsules. The lead enclosure will be installed in a hood to be built in the basement of the ORELA. ’General Engineering Division. ’Model A-9104 Dual Axis Rotator, commercially available from Kaman Nuclear Corporation, 1700 Garden of the Gods Road, Colorado Springs, Colo. 80907. 3F. A. Lundgren and S. S. Nargolwalla, “Use of a Dual 4E. Ricci, “Photon and Fast Neutron Activation Analysis at Sample-Biaxial Rotating Assembly with a Pneumatic Tube the Oak Ridge Electron Linear Accelerator (ORELA),” Anal. Transfer System for High Precision 14-MeV Neutron Activation Chem Div. Ann. Bog. Rept. Oct. 31, 1967, ORNL-4196, p. Analysis,” Anal. Chem 40, 672 (1968). 72. 63

n ,8:l.c Neutron Activation Analysis with a generators. It is small and free from power and ' Cf Source maintenance requirements; therefore, it is portable. Also, it permits the use of either pure fission neutrons Enzo Ricci T. H. Handley or a thermalized neutron spectrum and thus provides The hot cell and pneumatic transfer system f& use in the versatility needed in nondestructive analysis. Con- activation analysis with '"Cf spontaneous-fission neu- sequently, we studied the potential use of "'Cf trons has been completed at the Transuranium Research sources in field (geological or space) exploration for . Laboratory (TRL): also, a source of '"Cf was nondestructive analyses at the percent level. fabricated by the Transuranium Processing Plant and In view of this, our facilities are more versatile and installed inside the hot cell. Thus, it was possible to complex than the apparatus that will be required when carry out the first experiments of this joint program of this technique is finally used in the field. The 52 Cf the Chemistry and Analytical Chemistry Divisions. source is in a Teflon block (held by manipulator in Fig. A 25 Cf neutron source has rather unique character- 8.1). It may be transferred either to a dual-axis rotator istics compared with nuclear reactors and neutron for irradiations with fast neutrons (foreground) or to a high-density polyethylene cube for thermal- plus fast- neutron bombardments (background). A pneumatic 'E. Ricci and T. H. Handley, "Activation Analysis with a 252Cf Source," Anal. Chem Div. Ann. Progr. Rept. Oct. 31, transfer system shown schematically in Fig. 8.2 is used 1967, ORNL4196, p. 70. to deliver two samples at a time (unknown and

PHOTO 91358

a

Fig. 8.1. View of the Inside of the 2'2Cf Cell Through the Bromide Window. 64

ORNL- DWG. 68-3f46 Interesting conclusions can be readily drawn. First, it 0 is clear that the elements studied can be determined at percent or lower concentrations in 0.1- to 1-g samples. Second, although thermal-neutron activation is gener- ally very sensitive because of its higher cross sections, fast-neutron activation is a better choice in some cases. Therefore, it should be possible by selective activation with fast or thermal neutrons to minimize interferences . in nondestructive analysis. Calculations based on the above results show that a 4-ton truck can carry the shielding necessary for a 3-mg 252Cf source. Thus, a mobile unit for field exploration is envisaged that is capable of sensitivities better by a factor of 7 than that at which the above results were obtained.

8.1.d Influence of Channeling in Customary yI 5in. by 5in. NaI(TI) DETECTORS He Activation Analysis Enzo Ricci

The channeling of energetic charged particles in crystals has been known and studied since 1963.6 This LOADING - RECEIVING ~p“““““STATION, effect can be both beneficial and detrimental to charged-particle activation analysis of crystals. It was suggested recently7 that a quantitative measure of the fraction of impurities located on different lattice rows or planes can be obtained by bombarding a crystal Fig. 8.2. Schematic View of the ”’Cf Neutron Activation along different directions. On the other hand, a Analysis Facility. disadvantage of channeling is that it causes the particle range and the reaction cross section to vary in a rather complex fashion. Thus, when a crystal is irradiated in a channeling direction, the equations that govern standard) to the cell; an external switch directs the charged-particle activation analysis’ 79 do not hold; the samples to either of the two irradiation facilities. The mathematical interpretation of the activation experi- same system can take the samples from the cell either ment then becomes involved and uncertain. to a receiving station or to a counting setup. The latter When channeling is used to locate impurities in a can hold one sample between two 5 in. by 5 in. NaI(T1) crystal lattice, the sample is usually fDted to a rather detectors in an -477 geometry. sophisticated remotely controlled goniometer that We determined interference-free detection limits for activation analysis with fast and thermal neutrons for 12 elements of interest in geology and mining. By use %. Datz, C. Erginsoy, G. Leibfried, and H. 0. Lutz, “Motion of Energetic Particles in Crystals,” pp. 129-188 in vol. 17 of of the reaction 7Al(n,a)24Na, the neutron output of Annual Review of Nuclear Science, ed. by E. Segre, Annual the 252Cf source was found to be 8.6 X 10’ neu- Reviews, Inc., Palo Alto, Calif., 1968. trons/sec (+IO%) on March 10, 1968. This output 7D. M. Holm, W. L. Briscoe, J. L. Parker, W. M. Sanders, and corresponds to 0.37 mg of Cf. A cadmium ratio of S. H. Parker, “The Determination of 0 and C in Ge by 3He 8.3 was obtained for the reaction 7Au(n,y)’ 98A~in Activation,” Proceedings of the 2nd International Meeting on the high-density polyethylene cube. Detection limits Practical Aspects of Activation Analysis with Charged Particles, Liege, Belgium, 1967, EUR-3896d, f, e, p. 239. (mg) for a 1-mg Cf source follow. Those for thermal ‘E. Ricci and R. L. Hahn, “Theory and Experiment in Rapid, neutrons are: Na, 1.2;Al, 0.68; Mn, 0.075;Ni, 170;Cu, Sensitive Helium-3 Activation Analysis,” Anal. Chem. 37, 742 1.1; Zn, 83; Ag, 5.4; Pt, 86; and Au, 0.042. Those for (1965). fast neutrons are: Al, 13; Si, 2.3; Fe, 68; Zn, 68; and 9E. Ricci and R. L. Hahn, “Sensitivities for Activation Pb, 1370. The errors of these results are about +lo to Analysis of 15 Light Elements with 18-MeV Helium-3 Parti- *IS%. cles,”Anal. Chem 39, 794 (1967). 65

permits finding the channeling directions of the crystal The alignment of the (1 1 1) axis of the sample with the by irradiation. Thus, determination of concentrations as 3He beam was achieved by using a mirror mounted on low as ppb is ruled out, because high-intensity bom- the goniometer and an external autocollimator. The bardments cannot be attempted without cooling the irradiations were performed at the ORIC with a Y samples. To make cooling possible, the complexity of reasonably parallel 3He beam of 0.15 /.LAand 7.8 f 0.2 the goniometer must be increased beyond reasonable MeV. The channeling critical angle for bombardment of limits. under these conditions is 0.56 -I 0.01'. The objective of the 3He activation program at ORNL Thus, angle intervals smaller than 0.5" were used in the is to achieve the outstanding potential sensitivity of this irradiation of samples. A total of 18 samples were method. Therefore, the difficulties that channeling bombarded in sequence. Each was etched a short time effects may cause in high-intensity customary 3He before irradiation with conc HF-conc HN03 (1 : 2) for 1 activation analysis are of great importance to us and to 3 min. The bombardment angles (beam with respect deserve investigation. On the other hand, if these effects to (111) axis) were: -1.0, -0.8, -0.6, -0.4, -0.2, 0, were apparent in usual charged-particle activation, it 0.2, 0.4, 0.6, 0.8, 1.0, 4.0, 4.4, 4.8, 5.0, 5.2, 5.6, and might be possible to increase the sensitivity of the 6.0". The alignment was checked frequently with the lattice-impurity-location techniques. Thus, experiments mirror and autocollimator. were carried out to study these points. The nuclear reactions and products observed were: A single-crystal ingot of germanium (shaped like a 70Ge(3He,pn)7'As, 62 hr; 7oGe(3He,p)72As, 26 hr; margarine stick) was cut into numerous slices perpen- and 72Ge( He, 2n)' Se, 7.1 hr. A long-lived residual dicularly to its (111) axis. Each of these slices was activity, probably due to 18-d 74A~,was also present, bombarded at a different angle and counted. To ensure as well as 20.5-min ' C and 1 IO-min F from carbon the validity of the results over a wide area in charged- and oxygen impurities, re~pectively.~On the basis of particle activation, the sophistication of the experiment these half-lives, least-squares decay-curve analysis of the was planned to be greater than that of ordinary gross gamma counts (to improve precision) was per- bombardments and such that observation of channeling formed by using the CLSQ program in the IBM 360/75 I effect could be expected. However, since activation and computer . radioactivity measurements are standard in activation Figures 8.3 and 8.4 are plots of germanium product analysis, they were preferred to counting of prompt radioactivities vs angle. The error marks correspond to radiation. A simple goniometer accurate to +O. 1" was the standard deviations that result from the computer constructed to hold the samples during bombardment. treatment of the data. From the charged-particle activation eq~ation,~,9 the radioactivity induced in a

ORN L - DWG 68-6964 A io4 , I a I,I,, ,-_, I,,, I,I, 2- Zbhr. 72As

5 62 hr "As x 10 __

I

-1 2 -0.8 -0.4 0 0.4 0 8 4.2 4 6 50 5.4 5.8 RESIDUAL ACTIVITY ANGLE (degrees) :E (18d. 74As) IO -1.2 -0.8 -0.4 0 0.4 08 4.2 46 5.0 5.4 5.8 Fig. 8.3. Count-Rates of 72As and 73Se at End of ANGLE (degrees) Bombardment (E.O.B.) of Germanium Crystal vs Irradiation Angle. (Conditions: bombardment for 5 min with a 0.1-pA beam of 7.8-MeV 3He particles; counting of gross gamma Fig. 8.4. Count-Rates of 71Asand Long-Lived Tail (74As) at counts of sample on top of 1.3-cm lucite absorber lying on 3 in. E.O.B. of Germanium Crystal vs Irradiation Angle. (Conditions: by 3 in. NaI(T1) detector.) as for Fig. 8.3.) 66

thick target is proportional to the average cross section increase in the amount of pigment in the brain. Since of the nuclear reaction involved and to the particle this area of the brain has the propensity to concentrate range. If any of these variables were influenced by a number of cations, it was considered important to channeling in these experiments, Figs. 8.3 and 8.4 measure other metals in the basal ganglia of primates would show structure, that is, departure from horizon- after they were treated with phenothiazine. Copper as tal (constant). However, these graphs show that, within well as manganese is concentrated in biological pig- experimental error, the induced radioactivity is inde- mented tissues, and its clinical effects on the brain are pendent of irradiation angle. Despite the fact that this similar to those of manganese. Therefore, it was decided . study was set up with a much higher degree of optical to measure copper in addition to manganese in the alignment than is customary in charged-particle acti- various nuclei of the brain of our phenothiazine-treated vation analysis, its precision is not yet high enough for primates. detecting channeling effects. Thus, we can safely Neutron activation analysis was chosen as the method conclude that such effects cannot generally influence for measurement, because the amount of tissues avail- the customary methods. This is true particularly able for analysis is very small. The high concentrations because the critical channeling angle of 0.56" in these and good neutron cross section of sodium and experiments is relatively broad in comparison with that result in the production of 15-hr 24Na and 37-min corresponding to most activation bombardments. More- * Cl. The gamma-ray spectra of these nuclides obscure over, since channeling effects cannot be observed in an the peaks for 64Cu and 56Mn (Fig. 8.5). Girardi and experiment of medium sophistication as this one, it is Sabbioni' describe a radiochemical separation that apparent that fine studies of impurity locations by uses antimony pentoxide to remove sodium from channeling' will have to rely on complex equipment for activated samples. We used the technique and were able some time. Thus, no high-sensitivity determinations of to measure simultaneously both copper and manganese this type (requiring high currents) may be feasible in in our samples (Fig. 8.6). Table 8.1 summarizes the the near future. results. During these experiments valuable help was received A paper on this work will be presented orally.' from T. H. Handley and R. J. Fox.'

''Instrumentation and Controls Division. 8.1.e Trace Elements in Drugs ' 'Medical Division, Oak Ridge Associated Universities; pres- L. C. Bate ent address: Bowman Gray Medical School, Winston Salem, N.C. A cooperative program is under way with the Bureau 12F. Girardi and E. Sabbioni, "Selective Removal of Radio- of Drug Abuse Control through the Department of sodium from Neutron-Activated Materials by Retention on Hydrated Antimony Pentoxide," J. Radioanal. Chem 1, 169 Isotopes Development to determine the trace-element (1968). content of amphetamine and barbiturate drugs. Samples I3E. D. Bird, J. F. Emery, S. B. Lupica, and W. S. Lyon, (1 15) of the drugs were prepared and irradiated in the "Neutron Activation Analysis of Brain for Copper and Man- Bulk Shielding Reactor for one week. The induced ganese,'' to be presented at the 1968 International Conference, radioactivity was measured by both NaI(T1) crystal and Modern Trends in Activation Analysis, National Bureau of Ge(Li) diode spectrometry, and the decay was fol- Standards, Gaithersburg, Md., Oct. 7-11, 1968. lowed. The trace elements identified were Au, Br, Co, data are being processed to obtain quantitative results. 1 'q'I ' I ' I ' I ' I '

8.1 .f Neutron Activation' Analysis of Brain - Tissue for Copper and Manganese 24NO Me"-*& Me"-*& E. D. Bird' S. B. Lupica : -%e %+ %; - J. F. Emery W. S. Lyon 2% *.e'# 67

A

Table 8.1. Copper and Manganese in Brain Tissue of Phenothiazine-Treated Subhuman Primates

Putamen 9 32.4 f 5.4 2.05 f 0.24 1.88 f 0.31 Caudate I 32.7 f 3.7 2.05 f 0.19 1.81 f 0.08 Globus pallidus 8 25.2 f 7.5 2.05 f 0.28 2.09 f 0.23

'Dry-weight basis.

measurements and to make reasonable estimates of the responses of nuclides not previously measured. Preliminary experimentation has been completed. The relatively new Packard liquid-scintillation counter has been successfully interfaced with the Radiation Counter Laboratories multichannel analyzer. The sample-volume response of the detector system has been determined. As expected, the Cerenkov systems are very sensitive to sample volume. For example, I4C samples of volume from 1 to 20 ml exhibit an -5% variation in detection efficiency; 36C1 Cerenkov detection varies by a factor of -3. The shape of the experimental volume-response curve has already explained a questionable result in the literature. The shape of this curve can be developed Fig. 8.6. Gamma-Ray Spectrum of Eluate from a Chroma- tographed (Sb2O5 Column) Solution of Sample for Fig. 8.5. theore tically by consideration of the detector geome- try. 8.2.b Photovoltaic Conversion of I 8.2 NEW INSTRUMENTS AND TECHNIQUES Radioisotope-Decay Energy H. H. Ross 8.2.a Analytical Applications of Cerenkov Radiation The success of electrical power sources that use H. H. Ross thermovoltaic conversion of radioisotope-decay energy has already been adequately demonstrated. These Over the last year and a half, a number of papers have power sources have a number of advantages over appeared in the open literature that describe the use of chemical batteries; stability, reliability, and long life are Cerenkov radiation for radioisotope assay. The tech- notable examples. Recently, attention has turned to a nique is used primarily to measure energetic beta consideration of other forms of conversion processes emitters. A close study of these papers reveals some that can be used to exploit the decay energy of divergence of experimental results and the lack of a radioisotopes. Among the processes being evaluated, clear physical model for Cerenkov systems. photovoltaic conversion appears to offer a reasonable To resolve some of these difficulties, a program was alternate design concept for power sources with modest initiated to study in detail the Cerenkov process for electrical capabilities. beta-emitting nuclide assay. The initial phase of the Photovoltaic generation is, in fact, a two-step energy- program will involve a study of the experimental and conversion process. First, the radioisotope-decay energy theoretical variables that determine Cerenkov response. must be transformed into photon radiation having an After these results have been collected, attempts will be energy usually between 1 and 5 eV. This photon made to rationalize the discrepancies noted in the radiation is subsequently converted into electrical literature. Also, an experimental physical model will be power via a secondary converting element (silicon or developed to enable investigators to optimize their cells). 68

We have completed our program to evaluate the 8.2.e A Study of Parameters That Affect primary and secondary conversion processes and to Analytical Alpha Spectrometry study the emission characteristics of phosphors and the T. H. Handley J. H. Cooper14 factors that influence the fluorescent output of iso- Factors that affect alpha spectra were studied. They tope-phosphor combinations. The results of this pro- included uniformity and reproducibility of sources, gram can be used as the design basis for a radioisotopic counting conditions, and solids in sources. photovoltaic converter and will permit reasonable calcu- Standardization of these factors will be necessary lations to be made on the expected efficiency of many before computers can be used to resolve alpha spectra. converter systems. An open-literature publication that The results of this work will be presented at the describes the results is being prepared for submission to forthcoming Gatlinburg Conference.’ the International Journal of Applied Radiation and Isotopes. 8.2.f Low-Level Beta Detector 8.2.c Alpha-Radiation Damage in Inorganic J. F. Emery Phosphors The Physics Division was interested in determining H. H. Ross the resonance cross section of * Pb (Eo- = 0.6 MeV, tl12 = 3.29 hr). The expected disintegration rate was a A program to study the alpha-radiation damage in few disintegrations per minute per gram of Pb. To inorganic phosphors has been started at the request of detect beta decay of 0.6-MeV energy in a large mass of an interested government agency. The objective of the lead, the ratio of surface area to mass must be as large program is to determine the intensity and spectral as possible. A beta detector was designed with a total distribution of phosphors under continuous alpha bom- surface area of 183 cm2. Two 5-in.-diam multiplier bardment as a function of time. Phosphor-regeneration phototubes were attached to 1-mm-thick plastic scintil- techniques will also be evaluated. A specially designed lators by means of a quartz light pipe. The scintillators measurement instrument was constructed and tested. were covered with 1.5-mil-thick aluminum foil. The Also, an oversize glove-box assembly has been designed detectors were mounted face to face. Any coincident and is being fabricated. The box will be used to prepare counts were rejected, since they would be due to the isotope-phosphor sources and will house the major- cosmic activity. The background of these detectors ity of the detection and measurement equipment. mounted in this manner is 40 counts/min or 0.22 count min-’ cm-2 of detector surface. The efficiency for 8.2.d Quantitative Electrodeposition of I ‘Cs is 50%. Actinides from Dimethyl Sulfoxide T. H. Handley J. H. Cooper’ 8.2.g Liquid-Scintillation Counting of A simple, quantitative, and fast technique was devel- Weak-Beta Emitters in Aqueous Solution by oped for preparing sources for analytical alpha spec- Use of Triton X-100in an Organic System trometry by electrodeposition of radionuclides from dimethyl sulfoxide. In the presence of fluoride ion, S. B. Lupica americium(VI) is electrodeposited preferentially with The counting efficiency of weak-beta-emitting radio- respect to curium(II1). A decontamination factor of nuclides can be improved markedly by the incorpora- several hundred was obtained. It was also observed that tion of Triton X-100, -102, or -114 into the organic solutions of actinides in dimethyl sulfoxide low in scintillator system. Triton X is isooctylphenoxy- mineral acids were stable for at least two months. The polyethoxy ethanol that contains ethylene oxide results of this work were submitted for publication.’ (X-102, 12 to 13 moles; X-100, 10 moles; and X-114, 7 or 8 moles). It is a nonionic surfactant that improves

’4High-Level Alpha Radiation Laboratory. 15T. H. Handley and J. H. Cooper, “Quantitative Electro- 16J. H. Cooper and T. H. Handley, “A Study of Parameters deposition of Actinides from Dimethyl Sulfoxide for Use in Affecting Analytical Alpha Spectrometry,” to be presented at Analytical Alpha Spectrometry,” submitted to Analytical the Twelfth Conference on Analytical Chemistry in Nuclear Chemistry. Technology, Gatlinburg, Tenn., Oct. 8-10, 1968. 69

the solubility of water in the scintillator mixture Table 8.2. Liquid-Scintillation Counting Efficiencies without causing serious quenching (no energy lost to for 3H and I4C Achieved with Scintillator Systems That ionization). As a result 3H can be measured' in a Contained Triton X 6.55-vol % water solution with 22% counting efficiency Scintillator systems: toluene (0.7 1)-Triton component and in a 25-vol % water solution with 15% counting (0.3 I)-PPO (5.5 g)-dimethyl POPOP (0.1 g) efficiency. To compare systems, a figure of merit (FM) Amount of Counting is used; it is defined as the product of the volume Isotope Activity Triton Water Efficiency FM Component (~01%) # percent water and the percent counting efficiency (e.g., (dislmin) (%I 21.3 vol % water X 17.7% 3H counting efficiency = 376 = FM).' Table 8.2 gives the compositions of the 3H 4.79 X lo5 X-102 6.55 21.50 143 scintillator systems studied and summarizes the results. 9.53 16.67 159 13.60 18.07 246 More work will be done with solutions that contain <6.0 vol % water and less Triton X and with others that x-100 6.55 21.72 144 9.53 17.25 164 contain >20.0 vol % water; special attention will be 13.60 16.68 227 given to the use of Triton X-114. Other systems that X-114 6.55 21.43 143 incorporate other nonionic surfactants will also be 9.53 15.56 148 investigated. 13.60 17.65 240 14C 2.985 X lo3 X-102 11.78 79.30 934 8.2.h Low-Level-Radiation Counting Facility X-100 11.78 75.60 892 for Geochemical and Returned Lunar Samples X-114 11.78 78.00 920 J. S. Eldridge P. R. Bell' V. A. McKay' G.D. O'Kelley' R. E. Wintenberg'

Construction was completed on both the prototype PHOTO 90677 low-level-radiation counting system at ORNL and the final underground system in the Lunar Receiving Laboratory (LRL) at the Manned Spacecraft Center, Houston, Texas. The detector assemblies were put together according to the design criteria described previously.2 Experience gained with the prototype was valuable in making the final installation at the LRL. Figure 8.7 is a photograph of the final assembly at ORNL. The exterior of the shield, visible in the photograph, is covered by the outer anticoincidence mantel. Figure 8.8 shows the system opened for insertion of a sample; the upper detector and end-plug assembly are visible. The top section of the shield, with the anticoincidence mantel attached, rolls forward on a rail system. That section weighs -5000 Ib and can be opened easily with one hand.

''8. B. Lupica, Liquid Scintillation Counting of Weak Beta Emitters in Aqueous Solution Using Triton X-100,Jan. 8, 1968 (unpublished). "Chief of Lunar and Earth Sciences Division and Manager of the Lunar Receiving Laboratory, Manned Spacecraft Center, National Aeronautics and Space Administration, Houston, Tex. "Chemistry Division. 2oP. R. Bell, J. S. Eldridge, V. A. McKay, G. D. O'Kelley, and R. E. Wintenberg, "Low-Level-Radiation Counting Facility," Fig. 8.7. Photograph of Exterior of ORNL Low-Level Count- Anal. Chem Div. Ann. Progr. Rept. Oct. 31, 1967, ORNL- ing Facility. (The outer anticoincidence mantle that covers all 4196, p. 73. exterior surfaces is visible in this view.) 70

PHOTO 90680 Q

Fig. 8.8. View of Opened Shield and One of the Principal Detectors in the ORNL Low-Level Counting Facility. (The shield top-upper mantle assembly has been rolled forward for sample changing.)

Background measurements made with the prototype butions to the background are controlled. Two detec- detectors in the ORNL shield were only slightly greater tors were fabricated from the new spun cans. Prelimi- (

8.3 NUCLEAR PROPERTIES OF RADIONUCLIDES available for them. This agreement is much better than that of the 1966 intercomparison of Hg standardi- 8.3.a Interlaboratory Comparison of zations25 in which 50% of the participants reported Measurements of the Radionuclides values that differed by >lo% from the best values. * s7C0, 99Mo-99mTc,and 99mT~ Mercury-197 standards were not available at that time, and its decay scheme was in some doubt. J. S. Eldridge 8.3.b New Nuclear Data 4 Previous interlaboratory comparisons of radionuclide measurements2 were extended. The Subcommittee on J. F. Emery the Uses of Radioactivity Standards22 sponsored a test to compare concentration values determined at various Gamma-Ray Energies: - Variations in the reported laboratories for solutions of the radionuclides ’CO, values of the 2.16-MeV gamma ray from the decay of Mo-~ mTc, and 9mTc. R. C. Koch2 organized the 38Cl (ref. 26) and the 2.1 I-MeV gamma ray from the participation and sample distribution. Laboratories in decay of In (ref. 27) prompted the remeasurement the United States and Canada known to prepare or use of these energies. A high-resolution Ge(Li) gamma-ray these radionuclides were asked to participate and to spectrometer was used that has an energy resolution of report in detail their procedures for obtaining concen- 3.74 keV for the 2.75392-Mev gamma ray of 24Na. The tration values. Nineteen laboratories accepted the inter- energies of the single escape peak of this gamma ray and comparison samples, but only 13 submitted results. B. of the 2.6 1447-Mev gamma ray from T1 were used Kahn24 compiled the results and made detailed statis- as calibration sources; their respective energies are tical analyses. Two participants measured radionuclide 2.24292 and 2.10347 MeV. These energies were se- concentrations absolutely by 4n beta-gamma counting. lected so that the gamma-ray energies being measured Kahn took the mean values to be the “best” values. would be bracketed closely by peaks of known energy. Both the Nuclear and Radiochemistry Group and the The energies determined for C1 and In are 2.1668 Radioisotopes-Radiochemistry Laboratory measured ? 0.0004 and 2.1 122 k 0.0004 MeV, respectively. the samples received by ORNL; routine gamma spec- Thermal-Neutron Cross Sections. - The center hole in trometric techniques were used. Table 8.3 gives the the east D20 tank of the Bulk Shielding Reactor has a values reported compared with the best values. thermal-neutron flux of 1.2 X 10l2 neutrons cm-2 sec-’ . This facility was used to determine the thermal- Table 8.3. Results of Interlaboratory Comphnof neutron cross sections for the 4Ni(n,y)6 s Ni and Radionuclide Measurements - April 1968 c 208Pb(n,~)209Pbreactions. Dilute Au-AI alloy (0.100% Au) was used to measure the thermal-neutron flux. Concentration (pCi/g) Deviation Radionuclide The disintegration rate of 65Ni was determined by “Best” Value ORNL Value (%) NaI(T1) gamma-ray spectrometry; the 1.48-MeV gamma ray a ray disintegration 7c0 18.26 17.7 k 0.9 -3.1 of ‘’ Ni and gamma per value of 0.25 were used. The thermal-neutron cross section for 99~0 24.02 23.6 * 0.5 -1.7 99mTc 27.16 27.6 * 0.8 +1.6 64 Ni was determined to be 1.35 f 0.1 barns. The disintegration rate of Pb was determined by a It is interesting to note that every participant meas- 4n beta counter. The neutron source on the 4n beta ured all three radionuclides within 15% of the best mount was 50 pg/cm2. The thermal-neutron cross value. However, these radionuclides have been in section of 208Pb was determined to be 487 30 general use for several years, and standards have been microbarns.

21J. S. Eldridge, “Standardization of 197Hg,” Anal Chem 2s J. S. Eldridge, “Standardization of Mercury-197,” pp. Div. Ann. bog. Rept. Oct. 31, 1967, ORNL4196, p. 67. 313-322 in Standardization of Radionuclides (Proceedings of 22Subcomrnittee on the Use of Radioactivity Standards, the Symposium on Standardization of Radionuclides Held by Committee on Nuclear Sciences, National Academy of the Atomic Energy Agency at Vienna, October, 1966), IAEA, Sciences-National Research Council, 2101 Constitution Ave., Vienna, 1965. Washington, D.C. 20418. 26J. Van Klinken, F. Pleiter, and H. T. Di’kstra, “Beta and 23Member, Subcommittee on the Use of Radioactivity Gamma-Ray Measurements on the Decay of 38Cl,” Nucl. Phys. Standards. A112,372 (1968). 24Chairman, Subcommittee on the Use of Radioactivity 27C. M. Lederer, J. M. Hollander, and I. Perlman, Table of Standards. Isotopes, 6th ed., Wiley, New York, 1967. 72

8.3.c Applications of a BeWindow Ge(Li) Spectrometer System J. F. Emery

A Be-window Ge(Li) x-ray detector has been found to be a very versatile instrument. This device has been loaned temporarily to us by ORTEC and Bowman Gray Medical School. The efficiency for x-ray energies up to -100 keV is very good, whereas above -100 keV the efficiency decreases rapidly. Because of this difference in efficiency, it is possible to measure low-intensity x rays or gamma rays in the presence of high-intensity high-energy gamma radioactivity. By use of this system, it is possible to determine the highly converted 53-keV gamma ray (1 1%) of As in the presence of 72A~,74As, and 76As. An isotope product of 74As was found to contain I3As in l-pCi/ml concentration, whereas the "AS, 74 As, and 76As contents were 2.1, 10, and 0.6 pCi/ml, respec- tively. The 53-keV gamma ray of 73As could not be seen on an NaI(T1) spectrometer. Because of its high resolution, this detector is very useful for decay-scheme studies. For example, the 80-keV doublet associated with the decay of ' 3Ba can be resolved (Fig. 8.9). The separation of these two lines is only 1.340 keV, and the intensity of the 79.65-keV gamma is only 8% of the intensity of the 80.99-keV gamma. The resolution of this system at 81 keV is ." 0.700 keV. 270 280 290 300 310 320 330 CHANNEL NUMBER This x-ray spectrometer system was also used to study the gamma and x-ray spectra of '"I (Sect. 8.6.d). The 4 x rays plus gamma ray appear as a single peak on an Fi 8.9. Resolution of the 8@keV Doublet from the Decay NaI(T1) spectrometer, but they are easily resolved on of lf3Ba with the Be-Window Ge(Li) X-Ray Detector. this Ge(Li) x-ray spectrometer. The calibration of the efficiency of this detector deduced from energy sums, multipolarities, and intensi- involved a number of sources. Low-energy gamma-ray ties of the transitions. The quantum numbers of intensities of Am, Am, and N p can be nuclear-energy levels are associated with intrinsic and calculated from these data. These will be determined at collective modes of excitation in the framework of the a later date. Nilsson and Bohr-Mottelson models. Parameters rele- vant to rotational configurations and branching ratios 8.3.d Nuclear Spectroscopy in the Neutron- of the de-exciting transitions are evaluated. The energy Deficient 173

8.3.e Decay of 103Pd-103mRh the electron-capture branching to the 81- and 161-keV levels in Cs can be calculated. The absolute intensi- W. S. Lyon Marcia A. Lepri3 ties of the 356-keV gamma ray is highly dependent on An article on the decay of 103Pd-103mRhhas been any branching to these levels. The calculated electron- submitted to the Journal of Nuclear Medicine. A capture branching to these levels is negative; the limits summary follows: are -*2%. Since two Ge(Li) detectors were used at A radiochemical extraction was used to separate Io3Pd from different counting geometries, efficiency curves, and lQjrnRh and lo3Rh. The decay of Io3Pd directly to the calibrations, the errors were somewhat greater than lo3Wh state appears to be 100%. A new value was determined they should be. The ideal system for obtaining the for the K conversion coefficient of the 40-keV gamma ray of entire gamma-ray spectrum at one time is the Be- lo3mRh (1.8 f 0.2 X lo’), and the (&/Kp) ratio for window Ge(Li) detector. Use of this detector would K x rays (4.8 2 0.2) was redetermined. require a 4000-channel analyzer; the analyzer available 8.3.f Gamma-Ray Intensities in the Decay of ’ Ba for this work has only 400 channels. Table 8.4 summarizes the work. J. F. Emery Marcia A. Lepri3’

The large variation (52 to 74%) in the reported values 8.4 APPLICATIONS TO REACTOR PROGRAMS for the intensity of the 356-keV gamma ray from the decay of ‘”Ba prompted the investigation of the 8.4.a Precise Determination of ’ ’U decay scheme of 133Ba. A high-resolution Ge(Li) J. F. Emery spectrometer was used to measure the intensities of 100-keV and higher gamma energies; a Be-window Ge(Li) detector was used for the other gamma rays of Since the original study of the determination of ’ U energy below 100 keV (Sect. 8.3.c). by delayed-neutron co~nting,~’a need has arisen to The relative intensities and the absolute percentage of improve the accuracy and precision of the method for all known gamma-ray transitions were determined. All determining 235Uin MSRE fuel salt. This method is the gamma-ray intensities were corrected for internal also applicable to the determination of U. conversion by use of the values from Notea and Three innovations in the technique resulted in the G~rfinkel.~From the gamma-ray-transition intensities, improvement of the precision by a factor of 2. These were increasing: (1) the pressure of the air that propels 300RAU Student Trainee from Mt. Holyoke College, South the rabbit from 10 to 20 psi, a change that resulted in a Hadley, Mass. more reproducible decay time; (2) the duration of the 31A. Notea and Y. Gurfmkel, “Transitions in 33Cs From the irradiation from 60 to 120 sec; and (3) the decay time Decay of 133Ba,”Nucl. Phys. A107, 193 (1968). from 20 to 25 sec. Under these new conditions, the total count is somewhat less dependent on variations in the decay time. The S for sets of samples was decreased Table 8.4. Intensities of Gamma Rays from the from 0.5 to 0.3%, whereas the S for successive Decay of 133Ba irradiations of a single sample improved from 0.3 to 0.16%. Intensity ET (keW The lack of capability of the electronics of this Relative“ Absoluteb (%) system to handle extremely high count rates is still the 5 3.4 3.25 2.04 one single barrier to improving the accuracy of this 79.6 4.5 2.82 method. A new current-sensitive preamplifier has been 81.0 56.3 35.2 developed by the Instrumentation and Controls Divi- 79.6 + 81.0 60.8 38.0 sion that holds good promise. 161 0.72 0.45 223 0.63 0.39 277 11.4 7.14 303 29.0 17.8 356 100 6 2.6 384 14.4 9.0 32F. F. Dyer, J. F. Emery, and G. W. Ledicotte, A Comprehensive Study of the Neutron Activation Analysis of ‘Relative to the 356-keV gamma ray. Uranium by Delayed-Neutron Counting, ORNL-3342 (Oct. 2, bBased on 100 disintegrations. 1962). 8.4.b Proton Reaction Determination of Lithium source-to-detector distance of 15 ft). Pulse-height spec- and Fluorine in Molten-Salt-ReactorGraphite tra were taken with a 400-channel analyzer. Measure- ments were begun on March 28, 1968 (5 days after T. H. Handley J. H. Gibbons3 reactor shutdown), and were continued at intervals for R. L. MackIin3 Enzo Ricci 12 days. I D. R. C~neo~~ The fission products found in major amounts in the Prompt radiations from the reactions Li(p,r~)~Be and heat exchanger and fuel-salt-input and -output lines of l9F(p,q) l60 have been used to measure concentra- the heat exchanger were Nb, Mo, Ru, I, tions of the target nuclides ’Li and F in graphite; the and Te. Minor amounts of Ru and Ba-’ La ORNL 3-MeV Van de Graaff accelerator was the proton were found. The fission products detected in the pump source. A sample irradiated for nine months in the bowl and off-gas line included those listed above and MSRE shows more than a hundred times the lithium also ‘I, ’ 7Cs, and 41Ce. No 95 Zr was detected. and fluorine penetration found in an unirradiated The amount of each fission product deposited on the control sample. The results of this work have been heat exchanger increased slightly from the fuel-salt accepted for publication in Nuclear Applications. ’ entry point over about the first foot of heat exchanger and then decreased over the next 5 ft. Table 8.5 8.4.c Measurement by Ge(Li) Gamma Spectrometry presents the results. The value given in the last column of Fission Products Deposited in Components for each fission product was obtained by multiplying of the MSRE the value in the second column by the total metal surface area in the MSRE and dividing the resulting F. F. Dyer Robert Blumberg3 T. H. Mauney3 value by the total curies of that fission product in the An effort was made to determine qualitatively and MSRE at reactor shutdown. quantitatively the gama-emitting fission products that deposit on the components (principally the heat ex- Table 8.5. Major Fission Products Found in MSRE Heat Exchanger

changer) of the MSRE which came in contact with the ~~ fuel salt. This information is needed to estimate the Fission Product Deposited Mean Amount Fission on All Metal Surfaces of heat generated by the fission products after reactor Deposited Product the MSRE shutdown and for purposes of remote maintenance. (Ci/h2Ia Also, there is interest in the fission-product distribution (% of total in MSREP to determine whether correlations exist between the 95Nb 1.9 58 extent of deposition and such factors as temperature 99~0 4.9 102 ? gradients, molten-salt chemical effects, and half-lives of lo3Ru 1.1 64 fission-product precursors. In addition, there is a 13 2 Te-l3 2 I 2.2 66 specific interest in determining whether Zr deposits out. “Values pertain to heat exchanger only. bValues based on inventories of fission products calculated by The fission products were measured by gamma-ray E. L. and on total metal surface area in contact with spectrometry with a highly collimated Ge(Li) diode. the fuel salt as estimated by R. Th~rna.~~ The collimator consisted of a lead cylinder (1 9 in. diam, 33.5 in. length). The diode, in a small Dewar flask, was placed in a cavity in the top of the shield over a 8.4.d In-Reactor Penetration of Fission collimator hole (‘I8 in. diam, 12 in. length). By means Products into MSRE and Pyrolytic Graphite of the collimator, the detector could be focused on an L. C. Bate F. F. Dyer area (-3 in. diam) on the reactor components (a The Reactor Chemistry Division is being assisted in a study of in-reactor penetration of fission products into MSRE and pyrolytic graphite. Cylindrical specimens 33Physi~sDivision. were obtained by core drilling from blocks of graphite 34Reactor Division. removed from the reactor in the spring of 1967 and in 35T. H. Handley, R. L. Macklin, J. H. Gibbons, E. Ricci, and D. R. Cuneo, “Proton Reaction Determination of Lithium and March 1968. These specimens were sanded repeatedly Fluorine in Molten-Salt Reactor Graphite,” accepted for publi- to obtain samples on emery paper as a function of cation in Nuclear Applications. depth in the graphite. The thickness of graphite 36 Reactor Chemistry Division. represented by the samples was varied from -0.001 in. 75

near the surface of the specimen to -0.015 in. at a Chemistry Division. The microspheres are coated with depth of -0.5 in. graphite or silicon carbide. As the result of irradiation The first series of samples was measured by NaI(T1) and fuel burnup, the coating may crack and release spectrometry, the others by Ge(Li) diode spectrometry. fission products. c The improved resolution of the Ge(Li) diode permitted To measure the fission-product release under con- measurement of 95 Nb, Zr, ' ' Ru, ' O6 Ru, ' ' I, ditions that simulate in-reactor failure, microspheres are 132Te, 137Cs, 14'Ba, I4'La, 14'Ce, and '44Ce. irradiated to -15% burnup and allowed to decay for Resolution of ' Ce and ' 44Ce, ' ' Ru and ' Ru, several months. The 95Zr is then determined with a and Zr-95Nb was not possible by NaI(T1) spectrom- Ge(Li) diode to measure the percent burnup that oc- etry. It was observed that the concentrations of fission curred during the long irradiation. These data, along products decreased rapidly with distance into the with the irradiation history of the sample, are used to graphite. A significant finding was that for most calculate the U concentration in the original micro- samples the ratio of the disintegration rate of 95Nbto spheres. The microspheres are then reirradiated for 6 hr 95 Zr was about 10. Since the samples had decayed for to form measurable amounts of ' ' I and ' 'Ba-' La; several months, this fact indicates that 95 Nb penetrates the measured values are also used to calculate the ' U graphite much more readily than does 95Zr. The concentration. Next, the coatings of the microspheres surface sample of the pyrolytic graphite was very are cracked, and the microspheres are placed in an radioactive. However, at greater depths, the pyrolytic induction-furnace assembly. The furnace temperature graphite contained fission products in considerably for each run is 1100 to 1500°C. After 2, 8, 14, and 20 lower concentrations than did MSRE graphite. Also, hr of heating, the microspheres and furnace parts are ' 'Ba-l 'La was not detected in the pyrolytic graph- removed, and the ' ' I and ' 7Cs radioactivities are ite. measured to determine the rate and total amount of fission products released. The I3'I is determined di- 8.4.e Ge(Li) Diode Gamma-Spectrometry System rectly by Ge(Li) diode spectrometry and also indirectly F. F. Dyer L. C. Bate M. T. Morgan36 by calculation from the Ba-' 'La (1.60-MeV gamma peak) radioactivity measured by NaI(T1) gamma A 10-cc-volume Ge(Li) diode was obtained for high- spectrometry. The ' 7Cs is measured by NaI(T1) spec- resolution gamma-ray spectrometry. The detector is trometry. The release rates of ' 7l and ' 7Cs increase coupled to a Tennelec 135M low-noise preamplifier, as the temperature is increased; they are much higher which is coupled to a Tennelec 200 amplifier. A above 1400°C. Tennelec 250 biased amplifier is used to establish the Several of the microsphere coatings were removed 8 energy range of pulse-height spectra accumulated with a prior to heating, in which cases the coating and the core 400-channel analyzer. The data output from the ana- were heated separately. It appears that the release rate lyzer included punched paper tape, printed spectrum, is higher from the coating, although fission-product and both logarithmic and linear plots. The system concentration of the coating is about one hundredth resolution with the Ge(Li) detector is 2.5 keV for the that of the core. 1.33-MeV gamma ray of 6oCo.The photopeak counting efficiency for ' 7Cs at a source-to-detector distance of 10 cm is 1.1 X count per emitted photon 8.5 14-MeV NEUTRON GENERATOR compared with an efficiency of 7.0 X count per 8.5.a 14-MeV Neutron Generator Studies emitted photon for a 3- by 3-in. NaI(T1) detector. Spectral analysis has been accomplished mainly by J. E. Strain means of the data-reduction facilities incorporated in the analyzer. The system has been used primarily for Determination of Oxygen by 14-MeV Neutron Acti- vation. - The facility designed for the determination of analysis of fission-product mixtures (Sects. 8.4.d and oxygen in alkali and refractory metals has operated 8.4.0. routinely during the past year. Samples of lithium, 8.4.f Fission-Product Release from potassium, and calcium have been successfully analyzed Reactor-Fuel Microspheres for oxygen in concentrations as low as 19 ppm. Inter- L. C. Bate F. F. Dyer laboratory samples of lithium have been analyzed -to compare results obtained by vacuum distillation, The study of fission-product release from reactor-fuel thermal-neutron activation by the ' 0(3Yp)' F re- microspheres is a cooperative program with the Reactor action, and 14-MeV neutron activation. Work is con- 76

tinuing on the comparison of the determination of that diffuses into the target face as a function of target oxygen in potassium by 14-MeV neutron activation and temperature. A constant amount of available tritium is by amalgamation. The determination of oxygen in thereby maintained. This target is now being fabricated sodium by 14-MeV neutron activation is still under in- and should be available soon. vestigation as time permits. Conventional targets of titanium tritide and A large number of refractory metals (V, Nb, Ta, tritide are being analyzed routinely to determine the 8- Nb-lZr, Ni, stainless steel, etc.) have been analyzed by effects of fabrication techniques on their neutron yield means of standard additions. Oxygen is added in the and useful life. form of Mylar tape, of which oxygen is a component. The oxygen content of the tape is known from prior 8.5.d 14-MeV Neutron Reaction Research analysis, and the total oxygen added is determined by J. E. Strain weighing the tape. After the metal samples are activated and counted, a layer of the tape is applied to the sur- The Texas Nuclear Corporation model 9900 and the face of the sample, which is then reanalyzed. This Kaman Nuclear Corporation model 1250 neutron gen- method of standard addition permits the analysis of erators have been used in a variety of experiments to specimens that have irregular shapes. produce unusual radionuclides via the (n, h),(n,~), and Metal coupons used to test the compatibility of re- (n,p) reactions. Nearly all the experiments have been fractory metals with alkali metals are of a uniform sue. conducted in cooperation with members of the Physics, For these samples, standards are prepared by adding Health Physics, and Chemistry Divisions and with oxygen at elevated temperatures to form the oxides. ORAU students. The Kaman neutron generator is capa- The amount of oxygen added is determined from the ble of producing a flux of 14.7-MeV neutrons of 4 X weight gain of the specimen. A series of standard cou- lo9 neutrons cm-2 sec-’ ; the flux has a half-life of pons of Nb, V, and Ta have been prepared whose oxy- 2550 pA hr. gen contents range from 40 to >2000 ppm. 8.6 COOPERATIVE ISOTOPES PROGRAM 8.5.b Determination of Fluorine in Fluorspar by 14-MeV Neutron Activation Analysis 8.6.a Technical Assistance F. F. Dyer L. C. Bate S. A. Reynolds

At the request of the U.S. Bureau of Customs, the The joint program38 of the Isotopes and Analytical fluorine content of 15 samples of fluorspar ore was Chemistry Divisions in analysis and characterization of measured by 14-MeV neutron activation analysis. The isotopes has continued. Salient features of the program method of analysis was described previ~usly.~’ Dupli- are discussed either below or in cross-referenced sec- cate samples of each ore were analyzed. The average of tions of this report. The general program of the the results, converted to percent CaF2 in the samples, Isotopes Division is given in another rep~rt.~ was 1.06% higher than results based on a wet-chemistry method that were reported by the U.S. Bureau of Cus- 8.6.b Quality Control toms. This difference has not yet been explained. S. A. Reynolds 8.5.c Neutron Generator Target-Development The quality-control program will take into account Program standards for radiopharmaceutical raw materials. The J. E. Strain standards are under development by the Food and Drug Administration (FDA) with local cooperation. The In an effort to produce a tritium target for neutron anticipated FDA requirement for controls on raw generators that will produce neutrons at a constant rate, radioisotope materials - in addition to those on the a new concept in a self-regenerating target is under radiopharmaceuticals themselves - reflects an inter- study. The target contains a reservoir of gaseous 3H2 esting general attitude of users that isotopes should not

~ 38“Cooperative Isotopes Program,” Anal. Chem Div. Ann. 37L. C. Bate and F. F. Dyer, “Fluorine Determination by Prop. Rept. Oct. 31, 1967, ORNL-4196, pp. 81-86. 14-MeV Neutron Activation Analysis,” AmL Chem. Div. Ann. 39J. H. Gillette, Review of Radioisotopes Program - 1967, Progr. Rept. Oct. 31, 1967, ORNL-4196, p. 80. ORNL-4329 (in press, 1968). 77

contain any impurities. Expectations for radioisotopes analysis of the washings of the swabs for chlorine and are higher than those for chemical reagents, medicinals, chromium. No significant amount of chromium was and foods, for example. Some radioisotope users want found, andthe highest level of chlorine corresponded to assurance of purity rather than the customary guarantee 0.003 ml of sea water (it was probably the chlorine of replacement or adjustment if specifications are not from a fingerprint).

10 met. Examples of quality-control studies appear in the To evaluate a soil before heat-transfer studies, classi- following paragraphs and in Sect. 8.6.c. cal chemical and petrographic analyses appeared suffi- On Ba' C03 products, a discrepancy developed cient, as in a previous study.4 ' between isotopic-abundance values by radioactivity At the request of the Health Physics Division, a measurement and by mass spectrometry. One such routine method for tritium in water was reviewed. It occurrence in the past was caused by deterioration of a consists in distillation, followed by liquid-scintillation C standard, with resultant low radioassay. Current counting. It was confirmed that the method is reliable tests using the standard addition of National Bureau of in that the presence of other beta emitters would be Standards hexadecane-' C indicated that the radio- detected by the instrument and that satisfactory tri- assays are correct. Another past occurrence was be- tiated-water standards are available. Further, in connec- lieved to have been caused by Ba(OW2 coprecipitation, tion with a review for the American Public Health since C02 percentages were shown to be low; process Association of a procedure for tritium in water, doubt changes apparently eliminated the difficulty. The recent was expressed of the necessity of distilling all of a water difficulty was found by emission spectrography to be sample as prescribed. A cursory review of the literature caused by the presence of silicate material (glass and gave evidence that if half the sample were distilled, the possibly silicate). Such inert material does not bias of the measurement due to isotopic fractionation affect normal uses of the product. Sales have been would be <2.5%, and probably

publications and catalogs from other standards organi- within 2 to 5%, and the S of the isotope-dilution zations. A survey43 of the availability of and the analysis was -2%. The 'I abundance in the products criteria for standards was published. The criteria are was 85.3 to 85.7%. The spectrum of gamma and x rays essentially those covered in recent monographs? ,4 (Fig. 8.10) was taken by means of a Be-window Ge(Li) detector (Sect. 8.3.c). The K-conversion coefficient of 8.6.d Characterization of Isotope Materials the 40-keV gamma ray was calculated to be 10.6, and f the gamma intensity 7.3%, assuming theoretical ratios S. A. Reynolds J. F. Emery of conversion in other shells. Work remains to be done on measurement of specific activity. Preliminary data Experimental work on characteristics such as half- indicate that the accepted half-life of 1.6 X lo7 years lives, decay schemes, and cross sections of isotope will be approximately confirmed. materials continues as needed, and our compilation of A typical 1301 product was analyzed in detail. such properties is constantly updated. Some of the Impurities in very low levels (0.2% total) were found; information acquired will appear in the Zsotope Users' these included 1261, 1311, lZ2Sb,lZ4Sb, and lg7Hg. Guide, which is to be published by the Isotopes Information Center. This information has proven useful in local work in the Isotopes Development Center and Analytical and Health Physics Divisions and in our ORNL- DWG. 68-!2484 contributions to national organizations such as the ASTM. Some of the work is summarized below and in 5! Sect. 8.6.e. KU Work by W. S. Lyon and Marcia A. Lepri (Sect. 8.3.e) I and recent publications by others permit the following estimates for radiations from Rh: gamma, 0.07%; K x ray, 8%.The weighted average value for the half-life of "Fe is 44.6 days, in agreement with our value of 44.3 k 0.4 days, which we once thought was wrong. 5 The previous estimate of 0.06% for the intensity of the y1 0.022-MeV gamma ray of '"Sm was confirmed by new data. A mass of discordant data on Ba has been !O:i !O:i 2 published. The local work (Sect. 8.3.0 is definitive and should eliminate the major uncertainty in the assay and i application of this nuclide. W I- Work on the characterization of "'I is almost 3 complete; modern techniques have resulted in the z removal of past inconsistencies. The percentage of E CK activity carried by AgI was found to be >99.9%, and W the principal chemical components in typical products a v) were determined to be iodine and sodium, as expected. I- The chemical analyses for total iodine were confirmed z by using isotope dilution with known amounts of stable 40' 71, followed by mass spectrometry. Agreement was s 9

43S. A. Reynolds, "Availability of Standards for Common Radionuclides," Isotopes Radiation Technol. 52,118 (1968). 44B. Kahn, G. R. Choppin, and J. G. V. Taylor, Users' Guides for Radioactivity Standards, NP-17502, National Academy of 2t Sciences-National Research Council, Washington, D.C., 1967. 45S. B. Garfiikel, A. P. Baerg, and P. E. Zigman, Certificates 0 50 100 of Radioactivity Standards, National Academy of Sciences- CHANNEL NUMBER National Research Council, Washington, D.C., 1966. See also Certification of Standardized Radioactive Sources, ICRU-12 (Sept. 15, 1968). Fig. 8.10. Ge(Li) Spectrum of "'I. 79

The specific activity and the chemical and radionuclidic paper to be prepared jointly with G. I. Glea~on~~for punty of 91 Y were studied. The specific activity, based submission to Nuclear Science and Engineerin,p. Details on radiochemical and spectrographic analysis, was of the measurements for 99mTc are given here to found to be -2.3 X IO4 Ci/g (-95% of theoretical) as illustrate the techniques of determination, data treat- expected for fission-product ' Y. Traces of calcium ment, and selection and use of values from the and aluminum were found; the total solids (1 10°C) and literature. Portions of the mTc interlaboratory com- nonvolatile matter were 0.08 and 0.03%, respectively. parison solution (Sect. 8.3.a) were used for a determi- Our estimate of 30% 0.54-MeV gamma radiation in nation of the half-life of the nuclide. Pairs of samples 14'Ba, which is the same as that of ASTM Committee differing in radioactivity by a factor of two were E-10, was confirmed by measurements of that radiation measured repeatedly (1) for 1 1 half-lives by means of a from freshly separated barium, followed by measure- well-type NaI(T1) scintillation counter and (2) for eight ment of the well-known 1.60-MeV gamma in the ' 'La half-lives by use of a pressurized-argon 4n ionization daughter subsequently formed. In the ' 70rrmprogram, chamber. Data were analyzed by the CLSQ computer the heat output of Tmz03 wafers will be measured program, and no effects of impurity or other systematic calorimetrically. The theoretical heat production was errors were detected. Half-life results were: scintillation therefore computed. The value was 1.98 W/kCi, derived counter, 6.030 f 0.009 and 6.004 f 0.007 hr; ion from the average beta energy, 0.315 MeV, plus 0.020 chamber, 6.021 f 0.005 and 6.026 _+ 0.004 hr. MeV per disintegration for radiations associated with Uncertainties are standard deviations of least-square the gamma transition. A similar calculation was made fits. The unweighted average was 6.020 f 0.006 hr, and for ' 7Pm, based on the firm adoption by the ORNL the weighted average was 6.022 hr. Because of the range Nuclear Data Group of 0.0620 MeV as its average of the scintillation-counter results, the value will be energy. The corresponding heat output is 0.367 W/kCi published as 6.02.k 0.01 hr. This new value was com- or 0.341 W/g. bined with six others, and means were computed by -84 is produced by reactor irradiation of use of the AVERAGE program; two additional values enriched Sr ; the reaction is Sr(n,p)8 Rb. A typical were rejected as outliers. The recommended value is the product was analyzed for 84Rb by NaI(T1) gamma weighted mean, 6.03 hr, and the realistic uncertainty is spectrometry, by radiochemical separation, taken as equal to the standard deviation of the array, and others by Ge(Li) spectrometry. The observed *0.03 hr. intensity of the 1.90-MeV gamma in 84 Rb was -0.86% in agreement with 0.8% in Nuclear Data Sheets, but the 8.6.f Production of ' I for Medical intensity of the 1.02-MeV gamma was 0.3% vs 0.5%. Applications The 86 Rb content was 376, about as expected from the J. S. Eldridge H. B. Hupf4' J. E. Beaver48 (n,p) cross sections of 84Sr and Sr. Rubidium-83 was 0.7%, over twice as high as expected from the path Techniques were developed4 for the production of 84 Sr(n, 2n)8 Sr ' Rb, probably because of sub- ' I in quantity and of quality suitable for distribution stantial direct yield by 84 Sl(n,np)' Rb. The maximum as a new radioisotope product. Hundred-millicurie amount of *'SI was <0.002%. On the assumption that amounts of 1231were produced by the 123Te(p,n)1231 no separation of rubidium from cesium occurs in reaction in a 185-pA proton beam of the ORNL 86-in. chemical processing, the cesium content of the enriched cyclotron in a few hours by use of targets isotopically 84Sr target was estimated to be <2 ppm, from the enriched in ' Te. When highly enriched ' '3Te target absence of ' 34Cs in Ge(Li) spectra. The only nonisc- material was used, the amount of other longer-lived topic radionuclidic impurity detected was a trace iodine radioisotopes produced concurrently was 1.5% amount of 'CO. of the total ' I radioactivity, and the product was suitable for medical diagnostic use. Rapid separation 8.6.e Half-Life Measurements procedures for the product and target materials were S. A. Reynolds E. I. Wyatt4' J. F. Emery

Half-life values for 36 radionuclides were pub- 470ak Ridge Associated Universities. and values for -30 more will be included in a 481sotopes Division. 49H. B. Hupf, J. S. Eldridge, and J. E. Beaver, "Production of 46S. A. Reynolds, J. F. Emery, and E. I. Wyatt, "Half-Lives Iodine123 for Medical Applications," Intern J. Appl. Radia- of Radionuclides - 111," Nucl. Sci Eng. 32,46 (1968). tion Isotopes 19, 345 (1968). 80 developed. Half-life measurements gave a value of 13.02 not remove . This possibility was verified by f 0.02 hr for this nuclide. Spectral comparisons showed determinations of ’ 2Te in cation-exchanger inlet and that ’ 3mTe is a convenient and long-lived substitute exit and anion-exchanger exit samples, which show assay standard for ’ 31. negligible removal of tellurium by the cation exchanger and -81% removal by the anion exchanger. The prominence of 0.51-MeV gamma energies in the 8.6.g Special Analytical Assistance for spectra of the coolant-water samples prompted the Isotopes Development Center Activities identification of the nuclides that emitted this radia- tion. A decay plot was resolved into a long-lived J. S. Eldridge W. S. Lyon component (mostly I and ’ W), 10-min ’ N, and Numerous assays for a wide variety of developmental 110-min 18F. Interpretation of the 13N data is un- products were provided to various members of the certain because of the lack of knowledge about the Isotopes Development Center. Many of the samples behavior of nitrogen in HFIR. The level is inherently were incompletely processed products that contained reasonable, however, because use of the macroscopic radionuclide impurities which would interfere seriously cross section for 235Ufission neutrons, 13.5 X lo-’’ if routine assay procedures were used. Some samples cm-’ (ref. 52), gives -7 X 10’ ’ neutrons cm-2 sec-’ were checked for product purity; others were measured for the effective flux to which the water was exposed, for radionuclide content. The techniques of x- and compared with -10’ neutrons cm-2 sec-’ thermal gamma-ray spectrometry with NaI(T1) and Ge(Li) de- flux.50 Because of the removal of F- by the anion tectors were used. Samples that contained the following exchanger, the ratio of F to 3N was lower than that nuclides were assayed: 37Ar, 43K, 67Cu, 74As, predicted from their cross sections.’ 123mTe,1241, 1261, ‘291, lZ9Cs,13’Ba, 132Cs,and 181w 8.7 EFFECTS OF RADIATION ON ANALYTICAL METHODS 8.6.h Radionuclides in High-Flux Isotope 8.7.a Radiolysis of Radiation-Safeguard Reactor Coolant Water Spray Solutions S. A. Reynolds H. E. Zittel J. R. Lund’ The study of HFIR coolant water’ was continued in a minor way. At the request of the Operations Division, Study of the effects of radiation on radiation-safe- a method was devised for on-site monitoring of fission- guard spray solutions’ was continued. The results product release from fuel. The chosen method was obtained have been presented orally.’’ A summary of measurement of the 0.86-MeV gamma radiation of the paper follows. 52-min ’ 341 by gamma spectrometry in samples of the In a reactor accident, volatile fission products are effluent from the cation exchanger. A ’4Mn standard likely to be released to the atmosphere of the reactor was used; it was mounted in the same way as the containment. Radionuclides of iodine (largely ’ ’I) are coolant water samples. The same approach was chosen possibly the most likely radioisotopes involved and independently for monitoring fission-product release must be removed before the containment air is released from reactor-accident experiments.” Sample data to the atmosphere. It has been proposed that spray solutions be used as a means to sequester and fix such showed a rapid initial decay (I ’ Mo, ’ O4 Tc, etc.). The decrease in activity continued in a way which suggested that 1341 was supported in part by its parent 42-min ~~ ~~ ~ 4Te, as would be the case if the cation exchanger did ”L. Hammar and S. Forsen, “Formation of Nitrogen-13, Fluorine17 and Fluorine18 in Reactor-Irradiated H20 and D20: Applications to Activation Analysis and Fast Neutron Flux Monitoring,”J. Znorg NucL Chem 28,2111 (1966). ’OS. A. Reynolds and J. F. Emery, “Study of HFIR Coolant I/ Water,” Anal. Chem Div. Ann. hog. Rept. Oct. 31, 1967, 531nfraredand N.M.R. Group. ORNL4196, pp. 84-85. 54H. E. Zittel and J. R. Lund, “Radiolysis of Radiation- ’’ D. R. Wenzel, “Environmental Monitoring of Fission Safeguard Spray Solutions,” Anal. Chem Diu. Ann Progr. Product Release from the Loss-of-Fluid Test,” presented at the Rept. Oct. 31, 1967, ORNL-4196, p. 13. Symposium on Environmental Surveillance in the Vicinity of ”H. E. Zittel and T. H. Row, “Radiation and Thermal Nuclear Facilities (Health Physics Society), Augusta, Ga., Jan. Stability of Sprays,” presented at The American Nuclear 24-26, 1968. Society Meeting, Toronto, Canad, June 9-13, 1968. Q 81

airborne fission products. Accordingly, in the Nuclear depends on a variety of variables, for example, the Safety Program at ORNL the radiation and thermal amount of Oz available. The data of Table 8.6 indicate stability of such proposed sprays has been studied. what might occur in the real case, since the experi- It is estimated that these spray solutions will be mental conditions were selected to approximate reality. exposed to a maximum gamma-radiation dose of 1 X At a dose of 2 X 10’ rads, -1.4 volumes of radiolytic lo8 to 3 X lo8 rads accumulated over a period of Hz per volume of solution could be expected to form, weeks at temperatures that vary from room tempera- because the data indicate that the Hz generation is ture to -150’C. The stability of the spray solutions essentially a linear function of total dose. Variation of under these limiting conditions was determined. The the dose rate from 1 X lo3 to 1 X lo5 rads/min does solutions (all aqueous) studied were: not cause a significant change in the amount of Hz generated per unit of radiation. The possibility of the Identity Composition use of a “scavenger” to decrease the radiolytic genera- tion of Hz has been investigated. A-1 1 w/v % NazSz03, 3000 ppm B, 0.15 M NaOH, Thermal stability studies carried out in the absence of pH 9.2 radiation indicate that the acid thiosulfate solution A-2 3000 ppm B, 0.15 M NaOH, pH 9.3 A-3 H20, pH 6.2 (A-5) is completely decomposed at 140°C in less than A4 3000 ppm B, pH 4.6 72 hr and yields large amounts of sulfur, whereas the A-5 1 w/v % NazSz03, 3000 ppm B, pH 4.9 basic thiosulfate solution (A-1) shows

Table 8.6. Effects of Gamma Radiation on Group A Solutions‘

Gamma Radiation Change in I2 Apparent Hz Evolved Solution Dose (rads X lo-’) -APHz Equivalence (%) G(-SZO~~-) (cc/ml)c

1 1.00 0.1 2 1.87 0.2 2 0.12 2.81 0.3 0 0.24

I 4.74 0.4 -13 0.2 0.36 r 9.46 0.7 -4 2 0.3 0.70 2 10.00 0.1 0.69 4 10.00 0.1 0.12 5b 10.00 1.7 -97 0.6 0.70

A ‘Conditions: Volume ratio of gas phase to liquid phase, 25. Dose rate, 1 X lo4 rads/min. %.65 mg of sulfur per millimeter of test solution present after irradiation. ‘At STP. 82

in process and analytical work. The principal products silver was also included, because in most acids it forms a of the radiolysis of concern in chemical systems are passive surface that renders it immune to further attack. hydrogen and nitrite. Foils of the respective metals were cleaned and An example of the effect of nitrite is the decrease in weighed before being sealed into tubes with the acids. the amount of silver chloride formed from the chloride The acids were essentially air-saturated at the start. The produced by the radiolysis of chloral hydrate. The air-to-liquid volume ratio for each tube was roughly nitrite formed from nitrate in concentration of 0.1 M or 1 : 1. All samples were given gamma radiation doses of 3 more causes a visually detectable reduction of silver X lo7 to 5 X IO7 rads. The foil was washed, dried, and chloride to metallic silver. When the nitrate concentra- weighed after the irradiation to determine the amount tion is -0.01 M or less, this reduction cannot be dissolved. The acid was analyzed for the metal ion. The detected visually. No such reduction is observed in weight criterion of dissolution was set arbitrarily at 0.1 perchlorate medium, even at a perchlorate concentra- mg/cm2. Table 8.7 gives the results together with tion of 0.1 M or greater. previously reported results of irradiations in HCI. The slow attack on niobium by irradiated H2S04 was 8.7.c Radiolysis of Perchloric Acid unexpected. The mechanism by which this dissolution occurs has not yet been ascertained. Zirconium tends to Hisashi Kubota react with most oxygenated acids except HN03. This The radiolysis of perchlorate systems is interesting in immunity may be due to the formation of a passive film that there is reported to be very little reaction between that is not attacked by the radiolytically active species the primary products of the radiolysis of water and the present in this system; zirconium is even attacked perchlorate ion. The effects seen are principally “direct slightly by H3P04 to form a black surface film. effects” of the radiation on the perchlorate ion itself.’ The reports of all studies to date claim that chlorate Table 8.7. Solubility of Metals in Irradiated and possibly some chloride, is produced from the Mineral Acidsa perchlorate. Oxygen is another major product. Solubility Inb In the study of the possibility of dissolving some inert Metal HCl HN03 H2SO4 H3P04 HClO4 metals in irradiated mineral acids, the perchlorate acids were found to be colored yellow after irradiation, even Au + - - - + when there had been no interaction with the metal. A Ag + * + + + spectrophotometric scan revealed that the absorption Nb + - + ------spectrum of this yellow substance is the same as that of Ta W + - - - - C102. Further work has shown that this product is Zr + - d $* + indeed C102. No formation of C1- has been observed Pt + - - - - thus far. A post-irradiation effect occurs in irradiated per- =Conditions: foil weight, 0.1 to 0.4 g; foil area, 10 cm2; gamma radiation dose, 3 X to X lo7 rads. chloric acid. The amount of C102 in the acid following lo7 5 b+ = dissolution>O.l mg/cm2. - = dissolution

Hisashi Kubota 56D. Katakis and A. 0. Allen, “The Radiolysis of Aqueous Perchloric Acid Solutions,”J. Phys. Chem 68, 3107 (1964). The dissolution of the metals Au, Nb, Pt, Ta, W, and 57H. Kubota, “Dissolution of Some Inert Metals in Irradiated Zr in irradiated HCl was reported previ~usly.~~This Acid Chloride Solutions,” Anal. Chem Div. Ann. Progr. Rept. study was extended to the mineral acids in general, and Oct. 31, 1966, ORNL-4039, p. 10. 83

n Gamma radiation introduces a positive error in the iron-thiocyanate method. Invariably, the absorbance increases on radiation. In nonirradiated solutions, fad- ing occurs as a result of the reduction of Fe(II1) by the acid thiocyanate; gamma radiation reverses this effect. At a dose of -IO4 rads, the absorbance of the complex reaches a constant value; additional radiation up to lo6 rads does not increase the effect. In a sense, therefore, the radiation effect is desirable. The iron+,cu’-bipyridyl complex is fairly stable against gamma radiation. A dose of 2 X IO6 rads causes an error <1% in the determination of 2 ppm iron. At higher doses (lo6 rads), an increase in absorbance causes significant error. The increase is due to the products of the radiolytic decomposition of hydrox- ylamine which is present in large excess. The iron-], 10-phenanthroline complex is extremely stable against gamma radiation. If both blank and sample are exposed to the same radiation, very little error is caused by a dose as large as lo6 rads. This study indicates that, on the basis of effect of Fig. 8.11. Photomicrograph of AgCl Crystals Formed on gamma radiation only, the 1,lO-phenanthroline method Silver Foil by Gamma Irradiation in Concentrated Hydrochloric is preferred for use under conditions of high radiation. Acid. The results of this study were presented orallys9 and are being prepared for publication.

8.7.e Effect of Radiation on Common 8.7.g Studies Related to Project Salt Vault Analytical Reagents Hisashi Kubota H. E. Zittel Project Salt Vault has been completed except for a A chapter titled “Effect of Radiation on Common few post-demonstration studies. One item of interest is Analytical Reagents” was prepared for inclusion in the the residual moisture in the salt, both vertically and forthcoming book, Vol. 10 of SERIES IX, in Progress horizontally from the disposal hole. in Nuclear Energy.’ During the course of the demonstration Project Salt Vault, an abnormal amount of moisture came out of 8.7.f Effect of Gamma Radiation on each disposal hole. The amount was much greater than Spectrophotometric Methods for Iron was expected from the moisture content of the salt at the periphery of the hole. It was postulated that, as a H. E. Zittel result of a temperature gradient, moisture would move A study was completed to determine the effect of within the salt toward the region of higher temperature. gamma radiation in the more widely used spectrophoto- This postulation was made from calculations based on metric methods for determining trace amounts of theory.6 iron. The thiocyanate, a,a’-bipyridyl, and 1,l O-phenan- throline methods were evaluated to determine which is ,-.. preferable under conditions of high radiation. ’$ ”H. E. Zittel, “The Effects of Radiation on Some Analytical Methods,” presented at the Second Society of Analytical Chemistry Conference, Nottingham, England, July 15-19, ”H. E. Zittel, “Effect of Radiation on Common Analytical 1968. Reagents,” to be included in vol. 10, Remote Analysis of 6oR. L. Bradshaw, Health Physics Division, “Report on Joint Radioactive Materials, of SERIES IX, ANALYTICAL CHEM- Studies on Migration of Negative Crystals in Salt,” personal ISTRY, ed. by H. A. Elion and D. C. Stewart, in Progress in communication to Florentino Sanchez, ORAU Student Trainee Nuclear Energy, Pergamon, New York. from St. Edward’s University, Austin, Tex., August 1967. 84

After the removal of the radioactive elements from the region of maximum temperature (-200°C). The the demonstration holes, salt samples were taken at salt samples taken close to the hottest part of the various depths and distances away from the disposal heated holes did not shatter when heated up to holes and were analyzed for moisture. It was shown XOOOC, although they did lose some moisture. This definitely that moisture moved from the cold toward behavior indicated that all moisture initially present in the hot zones. There was some evidence of a steady- “negative crystals” had migrated and that the only state moisture concentration in the salt near the periph- moisture present was the transient moisture in the ery of the holes. This concentration was -0.1% near intercrystalline voids.

I/ 9. Inorganic Preparations D. E. LaValle R. B. Quincy

In a reduction of the fused-salts program, the prepara- continuation of work for the Neutron Diffraction tion of anhydrous rare-earth-metal halides for the Group, numerous rare-earth-metal alloys were heat- former High Temperature and Structural Chemistry treated, and the project to produce 50 g of 16’Gd by Group of the Chemistry Division was terminated, the the reduction of GdF3 with calcium metal was success- last salt prepared in this series being YbF2. For the Ion fully concluded. The preparation of high-purity KCl for Spectroscopy Group of the Metals and Ceramics Divi- the Research and Development of Pure Materials Group sion, however, work continued with the preparation of has been concluded. Work is now in progress to prepare such anhydrous materials as Ni(N03)2, NiC12, NiI2, high-purity MgO, about 20 lb of which has thus far NiS04, MgCl2, TiCI3, CuClz, LiN03, NaN03, KN03, been produced. LiCl, LiI, CsC1, and the eutectics KCl-LiCl and KI-LiI. For the Low Temperature, Nuclear, and Solid State A series of ferrites was prepared for the Neutron Physics Group of the Physics Division, further AuLi Spectrometry Group of the Solid State Division. The alloys were prepared in the range 0.25 to 0.50 at. % Au, ferrites are compounds of the structure Fe304 in which and, in addition, the alloy AuCa (0.7 at. % Au). For part of the iron is replaced by other metals. Examples another section of the same group, several intermetallic in this series are compounds were prepared: GeSe and GeTe, with both normal Ge and 73Ge, and the isotopic compounds 64NjAl and 61NiFe. Also, some compounds were prepared that contained nickel in various valence states: [(C6H50)3Pl4Ni (01, K4 [Ni2(CN)6] (I),K3[Ni(CN)41 For another section of the same group, samples of Ti0 (II), and KNiIO6*‘/2H20 (IC?. The methods of prep- and VO were prepared, and several attempts, only par- aration are described in the standard treatise Inorganic tially successful, were made to grow single crystals of Syntheses. ’Li. Other preparations of interest were ammonium azide In other work for the Solid State Division, high-purity (NH4N3) and beryllium nitride (Be3N,) for the Neu- ZnF2 and MgF, were prepared for the Lattice Defects tron Scattering Cross Section Studies Group of the in Halides Group, fused AgCl and sublimed LiI for the Neutron Physics Division. Also, the decontamination of Low Temperature Physics Group, and high-purity -7 kg of platinum was undertaken for the Stores MnF2 for the Lattice Defects in Oxides Group. In a Department. This project is about half completed. I . 44

VI rr VI 05 F N w w o I- w N Scientists e2 W m rrt4 cn P w I- P o m w r P Technicians U r Y m NUI- W W VI wcnm g Analyticalchemistry 0 +PO -N r wmI-m cnr N Biology M 4N VI 0 cn r W NW 4 m N "W "r "VI "W -+ Chemical Technology "P "OWLm N~N gggg # 4-w NWW -VIZ$ N+ w wl-P m w 00 P Q, VI Chemistry wwmm r w N rm - .. __ r r 01 00 4 4 Health mW m00 ~ 4N r 4w v,N +VI VI 4P w w row P Health Physics NW 0 P 4PU W - r r VI VI Inspection Engineering W r CJ P c N ch W w WOP m PPr "Q Isotopes PPN~N NW~+P 44ow r r.F.VI VIVI g we r e. W "VI "0 VI r "N .- g. m wm"w "a cc~"m Metals and Ceramics VIONW w VIOVI 1 .I wmw N OPP v,m e. v) -Y I r 2. P m4 Neutron Physics E6rZ00et.l I-- WWVI & (D< e 1 P VI 4 5' ow r cn rVI c Operations wm4m P no mow m rm z ? gw EcwVIVIr W & Physics w Pr + w NN N "P "I- w in "w 'tb Reactor rwmw 0 "3 0E P~WPw m4ca wr E W c w p w "W "e r N N W PwPw4 k mVI OWN0 'b eNN Reactorchemistry m4utm rn mu- ww cnr r e r m4 4 m 0 VI VIm r N 0 w Solid State -4 m cn o mm VI rw VI P OP004 Argonne National Laboratory W W P W WP General Biochemicals, Inc. c c W W N General Electric Co. 2 % M m Miscellaneous 0 I W wv, I Nuclear Fuel Services, Inc. I +I rl VI VI P 0 6 Other Plants

N N CU W Westinghouse Atomic Power W W Development Division

Total 4N ww i 86 ii 10. Methods Development and Evaluation L. T. Corbin P. F. Thomason

10.1 NEW METHOD FOR THE RAPID The eluent is a dilute aqueous solution of ff -hydroxyisobutyric SEPARATION OF BERKELIUM(1V) acid of pH 4.2. The eluted 249Bk is purified by extraction into FROM CERIUM(1V) BY ANION EXCHANGE 2-thenoyltrifluoroacetone-xylene. In this way the 249Bk is separated sharply from many elements including the actinides, F. L. Moore fission products, and corrosion products. Separations can be effected at eluent flow rates as fast as 18 ml cm-’ min-I, A new method was developed for the rapid separation thereby minimizing loading time, elution time, and radiation of berkelium from cerium. The simple method is based damage to the resin. High-pressure operation makes possible the use of a long column (“ 2 ft) having a small free column volume on the marked difference in the sorption of the anionic (“1 ml).” nitrate complexes of Bk(IV) and Ce(1V) on anion- exchange resins. Berkelium is separated quantitatively 10.3 NEW EXTRACTION CHROMATOGRAPHIC from cerium on small columns. The method is valuable, METHOD FOR THE RAPID SEPARATION because it functions in nitric acid solutions at room OF AMERICIUM FROM OTHER temperature and provides practical flow rates in glove- TRANSURANIUM ELEMENTS box or hot-cell facilities. The special case of an anion-resin column loaded with is particu- F. L. Moore larly attractive, because it eliminates a preoxidation For the rapid separation of americium from other step and introduces no solids into the solution. The transuranium elements, a new extraction chromato- method has several useful analytical and process appli- graphic method was developed. The work is described cations. in an article to be published: the abstract from which An article was published’ that describes this work. follows: “A simple, rapid method is described for the separation of 10.2 CHROMATOGRAPHIC-SOLVENT americium from curium and other actinide elements. The EXTRACTION ISOLATION OF ’ Bk FROM method exploits a new oxidation technique for the preparation HIGHLY RADIOACTIVE SOLUTIONS AND of americium(V) in dilute nitric acid solution with ammonium ITS DETERMINATION BY BETA COUNTING persulfate. Isolation of the americium is achieved by extraction chromatography with small Teflon columns containing di(2- L. G. Farrar’ J. H. Cooper’ F. L. Moore ethylhexyl) phosphoric acid as the stationary phase. The method considerably simplifies the purification and determina- A method was developed for the chromatographic- tion of 243Am in the presence of high levels of 244Cm. Several solvent extraction isolation of 249Qk from highly useful applications for both analytical and purification purposes radioactive solutions and its subsequent determination are discussed.” by beta counting. A paper on this work was published: the abstract follows: 10.4 THERMOGRAVIMETRICANALYSIS “A small high-pressure ion-exchange system has been used OF THORIUM IODATE together with liquid-liquid extraction to achieve decontamina- Canada tion sufficient to permit the determination by beta counting of D. C. 249Bk isolated from highly radioactive solutions. A high-pres- Solid thorium iodate, Th(I03)4, frequently contains a sure pump forces solutions through a column of Dowex 50 resin (20- to 40-p-diam particles) at pressures from 1800 to 2500 psi. large amount of absorbed moisture. The determinations of thorium, iodate, and water in this material were 0 IF. L. Moore, “New Method for Rapid Separation of requested. Since Th(I03)4 can be converted to the ! Berkelium(1V) from CeriumUV) by Anion Exchange,” Anal. oxide according to the equation Chem 39,1874 (1967). ’High-Level Alpha Radiation Laboratory. 3L. G. Farrar, J. H. Cooper, and F. L. Moore, “Chromate 4F. L. Moore, “New Extraction Chromatographic Method for graphicSolvent Extraction Isolation of Berkelium-249 from the Rapid Separation of Americium from Other Transuranium Highly Radioactive Solutions and Its Determination by Beta Elements,” to be published in the December 1968 issue of Counting,” Anal. Chem 40,1602 (1968). Analytical Chemistry. 87

-550°C measured by back-titration with EDTA. From this Th(IO3)4 -Tho2 + 212 + 502 , known value for a given weight of hafnium oxide plus the complete analysis can be done thermogravimet- zirconium oxide, simultaneous equations can be set up rically. The stripchart recording obtained in the ther- and solved for percent hafnium and percent zirconium. mogravimetric analysis shows sharp breaks at 100 and 550°C. Water is calculated from the weight loss at 10.8 BIOCHEMICAL ANALYSES 1OO”C, iodate from that at 550°C (212 + SO2), and D. C. Canada thorium from the total weight loss. A confirmatory iodate determination5 may be done volumetrically. The Analytical Biochemistry Group was assisted in the separation, identification, and determination of 10.5 GRAVIMETRIC DETERMINATION ribonucleic acids, deoxyribonucleic acids, proteins, lip OF TETRAFLUOROBORATE WITH MTRON ids, and polysaccharides. The results are discussed in Sects. 4.1 .b, -f, -g, and -h. D. C. Canada A sample of solid sodium tetrafluoroborate was 10.9 RAPID-SCAN POLAROGRAPHIC DETERMINATION OF URANIUM analyzed for tetrafluoroborate by a gravimetric nitron (C2oHI ON4) procedure.6 Nitron was purified by frac- P. F. Thomason tional crystallization from absolute ethyl alcohol. An alternate method’ that consisted in the partition The polarographic single-cell procedure and apparatus titration of tetrafluoroborate with tetraphenylarsonium previously described by W. L. Belew and co-workers’ chloride and amperometric end-point detection lacked was studied for the determination of uranium in MSRE the required precision and accuracy. fuel as a possible supplementary method to the con- trolled-potential coulometric titration method now in 10.6 DETERMINATION OF FLUORIDE use. With the ORNL model Q-2792 controlled-potential IN A MIXTURE OF dc polarograph-voltammeter, repetitive scans were ob- MOLYBDENUM FLUORIDES tained of standard solutions of uranium (5 X M) in various supporting electrolytes: 1.O A4 hydroxyl- D. C. Canada amine sulfate, 1.0 M H2S04, and 0.1 M HN03 that A mixture of solid molybdenum fluorides was anal- contained 0.001 vol % Triton X-100 as a maximum yzed for fluoride content. The best results were suppressor. Twenty five scans, each from tO.l to -0.8 obtained by pyrolysis followed by titration of the acid. V vs S.C.E., were obtained in -20 min. The peak An alternate null-point potentiometric method’ proved heights of the uranium first-derivative wave were to be somewhat inconsistent. measured by means of a digital voltmeter readout, and the average diffusion currents were corrected by sub- 10.7 DETERMINATION OF HAFNIUM tracting the average residual current. An unexplained AND ZIRCONIUM IN HAFNIUM decrease in the peak heights with time was obtained. OXIDE-ZIRCONIUM OXIDE MIXTURES This decrease was -1% more than the calculated electrolytic reduction of the U022+ ion. D. C. Canada The first results were encouraging, because an S of 0.1% was obtained for all the electrolytes. However, Determinations of hafnium and zirconium were re- when synthetic MSRE fuel samples that contained quested on hafnium oxide-zirconium oxide mixtures. known amounts of uranium were analyzed by the Total milliequivalents of hafnium and zirconium were standard-addition technique, a 1% negative bias in accuracy was obtained; also, the S was higher (-0.5%). r, ’R. Z. Bachman and C. V. Banks, pp. 331-32 in “Thorium,” -4 chap. 3 of Analysis of Essential Nuclear Reactor Materiuls, ed. by C. J. Rodden, Division of Technical Information, U.S. 8T. A. O’Donnell and D. F. Stewart, “Null-Point Potentie Atomic Energy Commission, 1964. metric Determination of Fluoride,” Anal. Chem 33, 337 %. A. Lucchesi and D. D. DeFord, “Gravimetric Determi- (196 1). nation of Boron. Precipitation as Nitron Tetrafluoborate,” ’W. L. Belew, M. T. Kelley, D. J. Fisher, R. W. Stelzner, and Anal. Chem 29,1169 (1957). E. S. Wolfe, “Investigation of Precision Attainable in Single-cell ‘K. Behrends, “Die Verteilungstitration von Tetrafluoro- First Derivative DC Polarography,” Anal. Chem Div. Ann borat,” Z. Anal. Chem 216, 13 (1966). Progr. Rept. Oct. 31, 1967, ORNL4196, p. 7. 88

The polarographic peak height of uranium is hydro- hanging drop of mercury. This unit will be used in the gen-ion dependent; the rate of disproportionation of stripping technique of analysis. U(V) to U(IV) and U(VI) is influenced greatly by the hydrogen ion. However, Verdingh and Lauerl found 10.1 1 CHARACTERIZATION OF TOBACCO that uranium peak heights become constant at an SMOKE AND SMOKE CONDENSATES HzS04 concentration of 1.8 N. Therefore, these low H. L. Holsopple results probably could not be due to the dispropor- tionation. W. L. Maddox' and D. R. Martin' recently In cooperation with the Lung Cancer Task Force of found that a D.M.E. controlled by a drop-knocker to the National Cancer Institute of the National Institutes 0.5-sec drop-time had an ac pickup from some source. of Health, the Analytical Chemistry Division has initi- This same type of trouble could have occurred while ated a program of research in the field of smoking and this study was in progress and accounted for some of health (Sect. 2.3). the erratic behavior encountered with the MSRE synthetic fuel samples. 10.1 1 .a Literature Survey When the ac pickup difficulty is eliminated and the apparatus becomes available, this study wili be con- As an initial step, a survey was made of the literature, tinued. and appropriate articles were collected and indexed for use by researchers in the program. It was found that a 10.10 THIN-FILM MERCURY ELECTRODE broad experimental and clinical approach to the subject VOLTAMMETRY OF BISMUTH has been manifest for the past few decades, the most extensive and definitive studies being undertaken since P. F. Thomason 1955. Although our chief interest is the analysis of tobacco A sensitive method is needed to determine bismuth in smoke, it was thought advisable to also obtain during MSRE fuel. A thin-film mercury electrode was prepared the literature survey additional articles on the use of by amalgamation of the platinum disk in an inlay style Beckman No. 1273 platinum electrode. This mercury tobacco and the resulting effects. It was hoped that this electrode was used to study the voltammetric determi- information would give the analytical researcher a nation of bismuth with the ORNL model 2792 con- broader view of the overall problem and, consequently, trolled-potential polarograph-voltammeter. a better idea of areas that need hs attention. However, For the polarographic determination of bismuth in since the scope of the problem is so large and includes urine, Lanza, Concialini, and Benati' recommend 1.0 such a great number of disciplines (this survey alone M EDTA-0.1 M NaOH as supporting electrolyte. It was gleaned 1200 articles from >200 journals), there is no found that in this medium bismuth gives a well-defined pretense that the collection is complete. wave at E1/Z = -0.65 V vs S.C.E. and that the diffusion The literature is assembled alphabetically and chrono- current is proportional to bismuth concentration over logically by journal in over 50 volumes. The journals the range 0.5 to 10 pg/ml. Interferences of materials in themselves are color-coded in five classifications: (1) the MSRE fuel will be studied. chemistry of tobacco and tobacco smoke, (2) medical - Also, the stripping technique (inverse polarography) general, (3) medical - neoplastic and cardiovascular, (4) will be studied as a way to increase the sensitivity of the sociological and psychological, and (5) general interest method. A Metrohm Micro-Mercury-Feeder E410 was or popular literature. For the chemist or biologist obtained to deliver uniformly and reproducibly a small starting research in ths area, the Analytical Chemistry Division's collection of tobacco-related articles and indexes should prove useful. "V..Verdingh and K. F. Lauer, "Accurate Determination of Microgram Quantities of Uranium by Direct and Differential 10.1 1.b Smoking Machine - Polarography," Z. Anal. Chem 235,311 (1968). ORNL $ "W. L. Maddox, personal communication to P. F. Thom- The first step in any smoke-characterization program ason, July 1968. is to provide a device for collecting samples under "ORAU Student Trainee from Sacramento State College, standard reproducible conditions. Such a device (Fig. Sacramento, Calif. 10.1) was constructed to smoke simultaneously six '3P. Lanza, V. Conciahi, and A. Benati, "Determination of Bismuth Content of Urine. Polarographic Method," J. Electre cigarettes at a rate of one puff per minute - a 35-ml anal. Chem 17,395 (1968). intake with a puff duration of 2 sec per cigarette. The 89

The acid and basic components of tobacco fractions were separated, and the test solutions were passed through gel-permeation columns. Further differentia- tion was thus accomplished. It is concluded tentatively that a gel-permeation technique for separating tobacco components should be a useful adjunct to gas chroma- tographic and mass spectrometric methods for the analysis of these fractions.

10.12 ABSORPTION SPECTROPHOTOMETRY OF ALPHA-EMITTING MATERIALS D. A. Costanzo The glove box and absorption-cell compartment designed for a Cary model 14 spectrophotometer14 have been used satisfactorily for the absorption spectro- photometry of alpha-emitting materials. The spectro- photometric method was used to determine americium Fig. 10.1. ORNL Smoking Machine. in the presence of curium, plutonium in the presence of zirconium, and ionic plutonium in the presence of polymeric plutonium. system has three traps for collecting the smoke conden- sates: one in an ice-salt bath at 0 to 1O”C, another in 10.13 MODIFIED WILLARD-WINTER isopropanol-liquid nitrogen at -40 to 5OoC, and a DISTILLATION METHOD FOR FLUORIDE third in liquid nitrogen at -195°C. This method of D. A. Costanzo collection provides an initial fractionation before the separations are made that are based on the solubility of The modified Willard-Winter distillation method’ the condensates in various solvents. was evaluated for the separation of microgram amounts To collect appreciable quantities of smoke aerosols of fluoride in acid nitrate media that contain moderate for gas-liquid chromatographic (GLC) analysis, 500 amounts of nickel, thorium, and bismuth. Over the cigarettes were smoked; 35 g of pyrolysis products was fluoride range 5 to 50 pg, the recovery was not less than produced. The results of GLC analysis are described in 95%. When present in the distillate, sulfate interferes in Sect. 2.3.a. the spectrophotometric determination with alizarin complexone.’ The sulfate interference can be mini- 10.1 1 .c Gel-Permeation Chromatography mized by the addition of sodium nitrate to the distillate as a Separations Technique prior to the addition of the chromogenic reagent.

Components of tobacco extracts were separated on 10.14 PRECISE DETERMINATION columns of Sephadex gels in both organic and aqueous OF URANIUM IN MSRE FUEL mediums. In the organic system, isopropanol was the solvent and LH-20 Sephadex was used as gel in a 2%- Gerald Goldberg by 100-cm column. At a flow rate of 50 ml/hr, The current method to determine uranium in MSRE components of both cigar- and cigarette-tobacco ex- fuel, that is, remote measurement by controlled-poten- tracts were separated on the basis of molecular size. In the aqueous system, a G-10 Sephadex column (1- Y by 100-cm) was used. Three different brands of cigars I4D. A. Costanzo and L. T. Corbin, “A Glove Box System for were agitated for 1 hr in water, and portions of the a Cary Model 14 Spectrophotometer,” accepted for publication filtered extracts were passed through the column. A in Nuclear Applications. comparison of the elution volumes of each of the ”H. Kubota, “Rapid Distillation Separation of Microgram Quantities of Fluoride,”Microchem J. 12, 525 (1967). resulting chromatographic peaks mp) of the three (256 16S. S. Yamamura, M. A, Wade, and J. H. Sikes, “Direct brands showed that each brand has essentially the same Spectrophotometric Fluoride Determination,” Anal. Chem 34, five major components. 1308 (1962). 90 tial coulometric titration in a solution of the fuel, has a PHOTO 91232 Q relative standard deviation (S) of -1%. For best control of the reactor by chemical analysis,. S should be no greater than -0.2%. Accordingly, a method is being developed that consists in the preliminary separation of the uranium from the remainder of the fuel by fluorination at 600°C and collection of the resulting UF6 in a trap of sodium fluoride. The contents of the traps is dissolved, and the fluorine is removed. The uranium, now free from interfering ions, is determined with a high-sensitivity controlled-potential coulometric titrator. To apply this method to highly radioactive samples that must be processed remotely in a hot-cell facility, special apparatus was designed and constructed (Fig. 10.2). The sample is melted from the ladle (seen hanging at the left) into a nickel liner within the reaction pot. The ladle and supporting flange are then replaced by a flange that contains the fluorine-inlet tube and gas-transfer line. The UF6 flows from the reaction pot through a pretrap of sodium fluoride at 400°C and then to the quartz collection trap. The excess fluorine is absorbed in the soda-lime-filled pipe. Nitrogen is used as a purge gas. To achieve high precision in the analytical procedure, it is necessary to remove the quartz collection trap from the hot cell. Since the fission-product radioactivity within the filled sample ladles exceeds 1000 rem, the Fig. 10.2. High-Temperature Fluorination Apparatus for the pretrap was incorporated to trap the bulk of the fission Recise Determination of Uranium in MSRE Fuel. products evolved during fluorination, for example, niobium, tellurium, and molybdenum. The UF6 is not adsorbed at 400°C. If the quartz trap is maintained at 1OO'C, the radioactive iodine passes completely between replicates of 0.1%. It is expected that uranium through the system. An S >OS% would be very recovery >99.5% will be achieved by adjustment of the difficult to achieve if it were necessary to dissolve, fluorine gas flow and flush rates. pipet, and titrate the sample within the hot cell. Several MSRE samples have been analyzed for ura- The apparatus has been installed in a hot cell. All gas nium. The gamma radioactivity within the quartz trap *. and temperature controls are located outside the cell after fluorination is <20 millirem; therefore the trap except the full-open and full-closed valves (Fig. 10.2). may be removed from the hot cell. A gamma scan of In preliminary tests, the recovery of uranium from the purified uranium sample showed that niobium is the standard samples has been not less than 97.5%. Coulo- major source of the radioactivity collected in the trap. metric titrations have been carried out with an S The total amount of niobium was <1 ng. i i i / 91

- 11. Spectrometry

A. E. Cameron

1 1.1 MASS SPECTROMETRY sections of the nuclides of that element. The laboratory participated in an interlaboratory check on a proposed 11.1 .a Transuranium Mass Spectrometry revision to ASTM method E-267, which is used to R. E. Eby measure uranium and plutonium concentrations and isotopic abundances in reactor fuels. The analysis of The Transuranium Mass Spectrometry Laboratory samples from the ' 71 Tm and ' Gd programs3 was reported 4136 results, about the same number as in the continued. previous year. Because of the addition of an analyst, the Seven samples of einsteinium were analyzed. No cost per analysis increased slightly, from $12.86 in difficulties were encountered except that each sample, FY-1967 to $13.80 in FY-1968. No one customer because of its radioactivity, ruined the electron multi- accounted for as much as a quarter of the analyses. The plier in the spectrometer. Some preliminary work has Isotopes and Chemical Technology Divisions continued been done to determine the relative values for the to be the principal customers. half-lives of the einsteinium nuclides. In collaboration with J. Halperin' and C. E. Bemis, .b Mass Spectrometry Services Jr.,' the partial alpha-decay half-lives of 24 F'u and 11.1 Pu were determined. The Pu alpha half-life was J. R. Sites determined by use of samples that were mixtures of E. J. Spitzer 239Pu and 242Pu. From mass and alpha spectral analyses and by use of the value 24,401.5 f 21.2 years The number of analyses reported by the Mass for the 239Pualpha half-life, the value 3.869 f 0.016 X Spectrometry Service Laboratory increased 20% from 10' years was obtained for the alpha half-life of 242Pu. last year. This increase includes a 5% increase in Similarly, mixtures of 244Pu and 242Pu were made, analyses for the Isotopes Division of isotopically en- and the value for the 244Pu alpha half-life was deter- riched samples of 46 elements. mined relative to the adopted value 3.869 f 0.016 x The relative isotopic abundances of several radioactive 10' years for 242Pu. The value 8.28 0.10 x IO7 solid samples were determined; the samples included years was determined for the 244Pu partial alpha those enriched in 36C1,40K, Ca, '"1, and 'I. half-life. The results of this work were submitted for In gaseous-sample mass spectrometry, certification publication.2 was continued of argon and helium contained in A similar program in which americium was used was cylinders and trailers, of nitrogen contained in cylin- conducted with C. E. Bemis, Jr.' Isotopic ratios of ders, and of the fission-product krypton and xenon various mixed standards of 24'Am and 243Am were that are prepared for sale. determined by mass spectrometry, and the data were Many sets of samples were analyzed for experimenters combined with counting measurements to determine who are studying such thmgs as gaseous cleanup, the relative half-lives. The data have not yet been contamination buildup in dry boxes, diffusion of gas analyzed. mixtures through membranes, and off-gases from the Other samples of interest include one from D. N. baking of various fuel pellets. Metta of Argonne National Laboratory. The plutonium collected from the decay of curium was analyzed to aid 11.2 EMISSION SPECTROMETRY (Y-12) in the determination of the half-lives of curium radio- J. A. Carter nuclides. Californium samples were analyzed for J. S. A. MacIntyre Halperin;' the results were used to calculate the cross The Spectrochemistry Laboratory reported about 47,000 results on 2500 samples, which represent 'Chemistry Division. 2C. E. Bemis, Jr., and J. Halperin,"The Alpha Decay Half Lives of Plutonium-242 and Plutonium-244, submitted to the 3R. E. Eby, "Transuranium Mass Spectrometry," Anal. Chem Journal of Inorganic and Nuclear Chemistry. Div. Ann. Progr. Rept. Oct. 31, 1967, ORNL4196, p. 94. 92 increases of 12 and ~WO,respectively. The Metals and .Table 11.1. Compounds Synthesized at ORNL That Ceramics Division was the largest supplier of samples Were Examined by Infrared Spectroscopy (26%). Many of these samples were experimental alloys Barium-p-ethylbenzenesulfonate submitted for composition analysis as well as for trace characterization. The Isotopes and Health Divisions Bicyclobu tane submitted about the same number of samples as last Boron nitride (vapor-deposited) Bromo-3-chlorocyclobutane year. Stable isotopes of the following 46 elements were 3Chlorocyclobutane carboxylic acid analyzed for trace impurities: Ag, B, Ba, Rr, Ca, Cd, Ce, Dimethylmonobutyl phosphate Cr, Cu, Dy, Er, Eu, Ga, Gd, Ge, Hf, Hg, In, Ir, K, La, Methyldibutyl phosphate Lu, Mg, Mo, Nd, Ni, Os, Pb, Pd, Pt, Rb, Ru, S, Sb, Se, 1-Methyl-4-thiouracil Si, Sm, Sn, Sr, Te, Ti, TI, W, Yb, Zn, and Zr. More than 1-Methyluracil 300 bismuth samples from the MSRE salt cleanup Silver 1-methylpyrimidine-4-sulfenate program were analyzed for thorium, lithium, and beryllium; the analyses were primarily for the Reactor Sodium l-methyl-2-oxo-pyrimidine-4-sulfenate Chemistry and Chemical Technology Divisions. Trimethyl phosphate

Fractions from compounds synthesized at ORNL 11.3 INFRARED SPECTROMETRY were examined for structure and purity (Table 11.1). M. M. Murray Materials produced by irradiation, chemical reaction, or other processes were identified. A summary of the The Infrared Laboratory has become increasingly results follows: irradiations of tall oil (a by-product of involved with the Body Fluids Analyses Program. paper production) and some of its fractions (oleic acid Preliminary investigation of a few of the materials and a sesquiterpene called caryophyllene); reaction known to occur in urine indicates that some are not mixtures from attempted syntheses of Na2LiF6; motor amenable to the treatment involved in the standard oils; pump oils; materials leached from the charcoal alkali-halide-disk technique. Since the major portion of filters of the Transuranium Processing Plant and of the the energy applied to the sample is transmitted during U.S.S. Savannah; SiF4 ; SiOF2 ; plastic tubing; an air the grinding of the sample together with the alkali sample from the Eagle Bend area near Clinton, Tenn.; halide, it was considered advisable to eliminate this step numerum column chromatographic samples from the if possible. Of the alternative methods considered, Body Fluids Analyses Program; and mixtures of Span lyophilization was the most attractive. Accordingly, a 80 and di-2-ethylhexanol. small “freeze-dry head” that uses liquid nitrogen as the Future work includes continued cooperation with L. refrigerant was designed, fabricated, and installed. Shop C. Brown’ in his investigation of the bromate-per- test of the instrument indicates that it can maintain a bromate system; acquisition of spectra of biological 5-p pressure under pumping. Laboratory test indicates compounds; investigation of a possible method of that it can reduce five 2-ml samples to satisfactory removing water from the alkali halide disk during the dryness in a short time (1 to 2 hr). The apparatus has pressing procedure, and investigation of the possible use seven ports fitted with commercially produced rubber of symmetrical difluorotetrachloroethane as an infrared valves. These valves fit a 16-mm-diam tube. Small solvent and/or mulling agent. samples can be lyophilized by freezing the sample in a small tube and inserting it in a 16-mm-diam tube; large samples, by using a flask having a 16-mm-diam neck. 1 1.4 NUCLEAR MAGNETIC RESONANCE A wide variety of organic and inorganic samples was SPECTROMETRY examined by infrared spectrometry. Most studies in- J. R. Lund volved the detection or identification, or both, of impurities in commercial products and in compounds Much of the nuclear magnetic resonance (NMR) . synthesized at ORNL; identification of commercial spectrometry has dealt with the elucidation of chemical products; characterization of organic compounds; de- structure and configuration of organic compounds that termination of impurities; or identification of structural resulted from studies by the Y-12 Organic Preparations changes in both organic and inorganic materials caused Croup. The NMR spectra, along with the mass (MA) by irradiation, chemical reaction, or thermal effects. and infrared (IR) spectra, were used to determine the 93

structure of such synthesis products as cinnamyl-

idenindene, diphenylbenzofulvene, dibromofluorene, Spectrometer and some isomers of truxene (Sect. 6.2). The spectra of Settings the simpler derivatives of indene, fluorene, and fulvene A B were very helpful in the elucidation of their structures. Filter band width, Hz I 2 Rf field, rnG 0.025 0.035 However, the truxenes are only slightly soluble in Sweep time, sec 500 250 solvents suitable for NMR spectrometry. The spectra of Sweep width, Hz 500 500 compounds of limited solubility were improved Spectrum amplitude 20 40 (<5%) Integrated amplitude 40 3.2 by use of a computer of average transients (CAT); Fig. 11.1 shows the improvement in the spectrum of a sample of truxene. Not only was the background noise reduced significantly, but the signals that result from proton absorption were enhanced considerably. Various polymers such as polymethylenepolyphenyl- isocyanate (PAPI), Varcums (polymers of furfuryl alcohol), organophosphorus polymers, and polymers of furan aldehyde were examined. Their NMR spectra indicate that most of them are mixtures; however, such groups as >P(O)H, >P(O)CH2 P(0) <, and ordinary alkyl groups were identified in the organophosphorus polymers. The spectra of the PAPI samples consisted of only two broad single peaks and indicated a ratio of aromatic to aliphatic protons of the order of 3 to 1. I I I I I I I Much more information was available from the spectra of the Varcums; they were found to be mixtures of furfuryl alcohol (I) and 5-furfurylfurfuryl alcohol (11) or of higher polymers of (I) and/or (11). Since the polymer of furfural is relatively insoluble in such usual NMR solvents as CDCI, or CCL,, attempt was made to measure the spectra of these polymers in such solvents as deuterodimethyl sulfoxide, (CD,), SO, and hexa- methylphosphoric triamide, ((CH,), N),PO at ambient Fig. 11.1. NMR Spectra of a Mixture of Trwene Isomers. and elevated temperatures. The attempts were unsuc- (Sample; saturated solution of truxene in CS2. NMR spec- trometer; Varian A60; -NMR spectra;- integrated cessful, because depolymerization occurred and the spectra.) A - one scan. B - 25 scans accumulated with the spectrum of the furfural molecule was observed instead. C-1024 computer of average transients (CAT); courtesy of The NMR spectra of numerous materials were re- Varian Associates, Instrument Division, Palo Alto, Calif. corded for the purpose of identification or comparison. Among these materials were hippuric acid; urea; caryo- phyllene; barium p-ethylbenzenesulfonate; and the four chemical shift of the signals due to angular methyl lipids estrololactone, '2&methyl-lPnortestololactone, groups in lipids reveals a great deal about the nature of and 2a- and 2@methyl-estra-4-ene-3,17-dione.) The the substituents and the stereochemistry of the rings. - 94

12. Process Analyses

L. T. Corbin

12.1 HIGH-LEVEL ALPHA A method was developed to determine bulk density RADIATION LABORATORY of large (about 1 X 4 X 8 in.) porous graphite blocks. The ranged from 0.8 to 1.6 g/cc. No liquid J. H. Cooper could be allowed to enter the pores, nor could the Over 23,000 results were reported by the High-Level samples be cut. Thin latex bags were made to hold the Alpha Radiation Laboratory. Most of these were for the samples. The samples were placed in the bags, and the Chemical Technology Division. Although the total bags were evacuated and sealed by a clamp. A sample personnel was decreased by 1076, the number of results volume was determined by immersing the bagged reported increased 17%. sample in a cylinder filled with water and catchng and A method for determining 249Bk was developed weighing the overflow. For samples of density <1, a (Sect. 10.2) and used routinely on samples from, the small piece of lead of known volume was placed in the Transuranium Processing Plant. This work is described bag with the sample. The S of the density measure- in a published article.’ ments was 0.1%. A method for determination of the oxygen-to-metal A small cylindrical pycnometer was constructed to ratio in Pu02-U02 pellets is now being used that measure the density of sections cut from HFIR fuel depends on changing the oxygen-to-metal ratio to plates. The volume of the pycnometer was 0.9 cc; that 2.000. A weighed portion of the dry sample is oxidized of the samples was 0.1 cc. The S of this method was in air at 850°C and then is reduced in a hydrogen-argon 0.5%. mixture at 850°C for 24 hr. The reduced sample is The arsenazo I11 colorimetric method2 for thorium assumed to be stoichiometric dioxide, and the change was used to determine thorium in bismuth metal. from the initial weight can be used to calculate the Thorium contents as low as 5 ppm were measured original oxygen-to-metal ratio. without separation of the bismuth. The S was 3% at the Samples of high-fired plutonia, mania, and mixtures 80-ppm level and 2% at the 1600-ppm level. of these with zirconia have been dissolved in sulfuric The American Public Health Association method for acid after a fusion in ammonium bisulfate. The fusion cyanide3 was used to determine cyanide in KCI crystals. can be done easily on a hot plate in a glove box. The No interference from the KC1 was encountered at sulfuric acid solution is in a form suitable for determi- cyanide concentrations of 0.2 ppm. nation of plutonium and/or uranium by coulometric The sealed-tube method was adopted for the dissolu- titration. tion4 of samples of uranium nitrides submitted for the Samples of LiF-BeF2-ThF4 salt have been submitted determination of nitrogen. This technique gave good for the determination of Th, Li, Be, Pa, Ni, Bi, and U.

Samples of bismuth that had been in contact with the ~~~ molten salt were submitted for the same analyses. The ’L. G. Farm, J. H. Cooper, and F. L. Moore, “Chromate salt samples are dissolved in nitric acid-boric acid and graphic-Solvent Extraction Isolation of Berkelium-249 from are fumed in perchloric acid to remove the fluoride. Highly Radioactive Solutions and Its Determination by Beta Counting,” Anal. Chem 40, 1602 (1968). The bismuth samples are dissolved in nitric acid. 2S. B. Sawin, “Analytical Use of Arsenazo 111, Determination of Thorium, Zirconium, Uranium and Rare Earth Elements,” Talanta 8,673 (1961). 12.2 GENERAL ANALYSES LABORATORY 3Standard Methods for the Examination of Water and W. R. Laing Wastewater Including Bottom Sediments and Sludges, 11th ed., ed. by L. Farber, pp. 356-58, American Public Health The work load in analytical biochemistry increased Association, American Water Works Association, and Water Pollution Control Federation, 1960. 48%; the total number of determinations of tRNA was 4G. W. C. Milner and I. G. Jones, Improvements in the 69,996 compared with 46,464 last year. For this Determination of Nitrogen in Plutonium Mononitride and analysis, the average cost per analysis was reduced from Uranium Higher Nitrides by Chemical Methods, AERE-R-5329 $1.89 to $1.62. (November 1966). 95

nitrogen results, but when the samples were heated at Those items of interest can be photographed with a 195”C, as specified, dissolution sometimes required camera especially fabricated for attachment to the several days. A recently translated Japanese article’ periscope. 4 describes the effects of the additions of oxidizing agents Equipment for fluorinating the uranium from 50-g on the dissolution of boron nitride. Forty milligrams of samples of MSRE fuel salt was installed and tested in a KC104 was added with the 9 N HCI to dissolve a 0.2-g work cell. The fluorinated products will be further sample aliquot. Dissolution time was reduced from treated and then measured for uranium isotopes pres- several days to 4 to 16 hr at 195°C. When KC104 was ent. The apparatus will also be used to improve the used, it was necessary to add Devarda’s alloy for the measurement of the uranium concentration in fuel-salt ammonia distillation to recover all the nitrogen. samples from the MSRE. A Laboratory Equipment Corporation Nitrox-6 ana- A chapter titled “Sampling, Sample Dissolution,

lyzer was modified for the determination of oxygen in Evaporation, and Combustion ” was completed for uranium nitride. A column of hot copper oxide was inclusion in Vol. 10 of SERIES IX, Progress h Nuclear added to oxidize the in the furnace Energy.6 exit gas to carbon dioxide. The molecular-sieve gas- chromatographic column was replaced by a column that 12.4 RADIOISOTOPES-RAD1 OCHEMISTRY contains silica gel. The molecular-sieve trap was oper- LABORATORY ated at room temperature. These modifications allow the nitrogen released from the sample to pass through E. I. Wyatt the analyzer with the carrier gas. The small amount of The types of work performed in the Radioisotopes- oxygen present can be measured without interference Radiochemistry Laboratory have remained essentially from the large amounts of nitrogen gas. unchanged for the past two years. The total volume of Moist-oxygen pyrolysis with Na2 W04 W03 flux was analyses was only about 75% of that of 1967. This used to determine fluoride in MoF3 and MoF,. decrease was due primarily to a reduction of the funds The total number of results reported increased from available to the Chemical Technology and Reactor 99,125 to 11 1,623. Chemistry Divisions. New equipment put into service includes an IBM 12.3 GENERAL HOT-ANALYSES LABORATORY card-punch machine, a 4096-channel pulse-height ana- C. E. Lamb lyzer, and a flame spectrophotometer. Cell 5 of the HRLAF (Building 3019) was cleaned and put into Interest continued for essentially the same analytical service, and cell 7 was cleaned and stripped and is out services required last year. A total of 19,834 reported of service. results reflects a 4% increase. The largest part of our radiometric analyses were The recently installed glove-box facility was used performed in support of the Fast Breeder Reactor Fuel extensively in the measurement of solid samples for gas Processing Program of the Chemical Technology Divi- release, density, carbon, surface area, and oxygen. The sion. Almost all these analyses were done by computer samples analyzed were’ received mainly from the Chem- resolution of gamma-ray spectrometric data. Another ical Technology and Metals and Ceramics Divisions but large block of work consisted in the dissolution and also from customers outside ORNL, namely, Argonne subsequent radiometric and radiochemical separation of National Laboratory, Vallecitos Nuclear Center, and various samples from the core and pump bowl of the Nuclear Fuel Services. The gas-release equipment is MSRE. to 1800°C from the previous being modified for use up The half-lives of 36 radionuclides were reported (Sect. limit of 1200°C. 8.6.e).’ Decay-scheme data were collected for all A Kollmorgen periscope with 2X, 4X, lox, and 20X radionuclides that have a half-life of 1 min or longer magnifications was installed through the wall for viewing within the storage cell. With the periscope, samples or unique materials can be examined visually. 6C. E. Lamb, “Sampling, Sample Dissolution, Evaporation, and Combustion,” to be included in vol. 10, Remote Analysis of Radiaactive Materials, of SERIES IX, ANALYTICAL CHEM- ISTRY, ed. by H. A. Elion and D. C. Stewart in Progress in 5S. Nakamura, N. Azuma, and Z. Arai, “Decomposition of Nuclear Energy, Pergamon, New York. Boron Nitride with Acid and the Effects of Some Oxidizing ‘S. A. Reynolds and J. F. Emery, “Half-Lives of Radio- Agents,” Kogyo Kagaku Zasshi 63, 903 (1960); ORNL-tr-1242. nuclides-111,” NucL Sci Eng. 32,46 (1968). 96 and also gamma radiations of 50 keV or greater. A 12.6 QUALITY CONTROL computer program was written to list the data in readily G. R. Wilson accessible form for qualitative Ge(Li) spectrometry. Also, a computer program for the quantitative resolu- The fxed 2s values of the control programs that have tion of Ge(Li) spectra is almost completed. been in operation for over a year remained at the same Many LiF-BeF2 salt samples were analyzed for trace level. The 2.8% decrease in the quality level for the past quantities of europium, lanthanum, and by year is due to the newly initiated control programs neutron activation analysis. These samples were sub- whose 2s limits are not yet established. mitted in aqueous solutions and were irradiated in the Several new control programs were established. The air-cooled HB-5 facility in the LITR at a flux of 5 X General Hot Analyses Laboratory now has a control 10' ' neutrons cm-2 sec-' . Under the conditions of the program for the determination of plutonium in the experiment, the detection limits were 1, 10, and 6 ppb presence of uranium by coulometric titration. Control for europium, lanthanum, and neodymium, respec- programs for the following determinations are now in tively. A similar technique was used to determine ' I operation in the General Analyses Laboratory: flame to a limit of 20 ppb by use of a flux monitor instead of photometric lithium, dibenzylmethane colorimetric ura- a standard. nium, and arsenazo 111 colorimetric thorium; the last three determinations are done in the presence of 12.5 RADIATION CONTROL AND SAFETY bismuth. The High-Level Alpha Radiation Laboratory has new control programs for coulometric titration of C. L. Burros plutonium, dibenzylmethane colorimetric uranium, and The absolute filters in the off-gas system at the arsenazo I11 colorimetric thorium; the last three are run HRLAF (Building 3019) were replaced and tested. The in the presence of bismuth. containment liner in cell 5 was dismantled and placed in The decrease in the total number of control results is a plastic-lined coffin. After the lid was secured, the due to fewer samples from the MSRE. The quality level coffin was wrapped with plastic and then moved to the by laboratory is shown in Table 12.1. burial ground. Cell 5 was decontaminated and painted. The 8-ft hood in the southwest zone was moved to the Table 12.1. Distribution by Laboratories burial ground, and the air conditioner was relocated to of Control Tests for July 1967-June 1968 permit the installation of an air lock. These jobs were Number of completed with minimum spread of contamination and Control Results Quality

~ Level(%)' exposure to personnel. Laboratory Outside On July 15, construction of the West Annex to Total Fixed 1967 1968 Building 2026 (HRLAL) was begun. Limits The annual safety inspection of all work areas in the Division was made with a safety engineer July 9-12. General Hot-Analyses 1235 121 93.89 90.20 General Analyses 2022 131 95.75 93.52 This inspection included checks for such items as poor High-Level Alpha Radiation 29 11 62.07 housekeeping, defective electrical equipment, unsecured - - -- Total 3286 263 94.82 92.00 gas cylinders, unguarded mechanical or experimental equipment, improper storage and use of flammable aControl results within prescribed 2s limits. liquids, lack of use of protective personal equipment, or any unsafe conditions. A written report on the inspec- The number of control results and their specific tion was made to the Division Director. Twenty-one medical-treatment injuries wefe reported for the past characteristics are given in Table 12.2. 12-month period. Most of these were hand injuries due to glass breakage. On several occasions, safety films were shown at Buildings 2026 and 4500s for employees of the Division. 97

Table 12.2. Distribution by Methods of Control Results for July 1967-June 1968

Number of Number of Type of Method Constituent Control Programs Control Results

Amperometric Chromium 1 147 Zirconium -1 2 119 266 Colorimetric (Spectrophotometric) Aluminum 1 53 Chromium 1 118 Iron 2 35 7 Molybdenum 1 38 Nickel 2 28 1 Thorium 4 219 Uranium -4 15 223 1289 Coulometric titration Plutonium 2 41 Uranium -3 5 950 991 Flame photometric Lithium -1 1 -72 12 Fluorometric Uranium -2 2 283 283 Gravimetric Carbon -2 2 202 202 Photoneutron Beryllium 1 1 80 80 - - Polarographic Uranium 1 1 83 83 - Volumetric Aluminum 1 1 20 20 - - - - Total 30 3286 .

Part C. ORNL Master Analytical Manual

13. ORNL Master Analytical Manual

M. T. Kelley Helen P. Raaen

13.1 CUMULATIVE INDEXES TO THE Altogether, five new methods were added to the ORNL MASTER ANAL YTICAL MANUAL Manual; one of these was for the purpose of record only. Revisions were made to six methods. (See The cumulative indexes to the ORNL Master Analyti- “Presentation of Research Results.”) The status of nine cal Manual were not updated in 1967. However, they methods for the Transuranium Process was changed will be in 1968 to indicate changes made in the content from tentative to formal. of the Manual during both 1967 and 1968. A survey was made to determine what methods now contained in the Manual are no longer used, what 13.2 MAINTENANCE OF THE ORNL MASTER revisions to existing methods are needed, and what new ANALYTICAL MANUAL methods are required for current or anticipated ana- No supplement to the reprinted form of the ORNL lytical work. On the basis of the survey, method-writing Master Analytical Manual was published in 1967. The assignments were made to persons in the Analytical tenth supplement will be published in 1968 and will Chemistry Division. contain the new methods and revisions issued in both 1967 and 1968.

98 Part D. Activities Related to Educational Institutions

14. Activities Related to Educational Institutions

Certain activities come into existence when the interests, purposes, and problems of educational institutions and of the Oak Ridge National Laboratory overlap in the area of analytical chemistry. The more formal of these activities include discussions with consultants who are also university faculty members, and thesis-research programs for graduate students. By less formal arrangements, faculty members engage in research in the Division under the ORAU-ORNL Research Participant Program, and students participate in the Summer Student Trainee Programs and in the Loanee Program for special work. Often,, a number of the Alien Guests in residency for work in the Division are from foreign educational institutions or from foreign laboratories whose programs intersect those of educational institutions. The nature and the mutual benefits of these activities are indicated throughout this report. Of the approximately 125 formal presentations of the research of the Division made during the past year, about 10% reflect cooperative ventures with educational institutions. These presentations are enumerated in the “Presentation of Research Results” section, and the work is discussed in the sections of the report indicated.

14.1 ADVISORY COMMIlTEE MEMBERS AND CONSULTANTS

The Advisory Committee members and consultants who have worked under subcontract in collaboration with our division are: J. A. Dean M. L. Mo&* University of Tennessee Institute for Muscle Disease, Inc. H. A. Laitinen* A. 0. C. Nier University of Illinois University of Minnesota Gleb Mamantov L. B. Rogers* University of Tennessee Purdue University G. H. Morrison* Cornell University *Advisory Committee Member.

14.2 ORAU RESEARCH PARTICIPANTS Two ORAU Research Participants were with us in the summer of 1968. a J. C. Guyon, Professor of Chemistry, University of Missouri, Columbia, worked with W. D. Shults, Methodology Group, to investigate the voltametric and coulometric behavior of plutonium, neptunium, and americium in their various oxidation states in several aqueous media (Sect. 2.7.d).

99 100

C. R. Spell, Chairman, Department of Chemistry, Emory and Henry College, Emory, Va., worked with D. J. Fisher, Analytical Instrumentation Group, to survey the dc polarographic characteristics of urinary-constituent biochemicals that are chromatographically separated in the ORNL Body Fluids Analyses Program and to assess the feasibilities of using dc polarography for the qualitative and quantitative monitoring of column effluent streams and Y for laboratory identification and concentration analyses of biochemicals in column fractions (Sect. 1.8). An S Contract Holder under the ORAU Participation Agreement worked with us from July 21 through August 3. T. T. Davies, Assistant Professor of Geology, University of South Carolina, Columbia, worked with H. W. Dunn in the X-Ray and Spectrochemistry Group to evaluate the electron microprobe for use in studying the concentration of stable elements in skeletal material of benthic invertebrates collected on the West Coast of Puerto Rico. This work was a continuation of work he began in the summer of 1967 at the Puerto Rico Nuclear Center.

14.3 GRADUATE THESIS RESEARCH PROGRAMS 14.3.a ORAU Graduate Fellowship Program H. W. Jenkins, a graduate student in the Department of Chemistry with Professor Gleb Mamantov at the University of Tennessee, Knoxville, is continuing his work toward the Ph.D. degree. In the Reactor Projects Group with J. C. White and D. L. Manning, he is studying reference electrodes in fluoride melts to develop a practical reference electrode. Also, he is investigating the behavior of several metallic couples with the objective of establishing an electromotive series for fluoride melts (Sect. 3.2.~).

14.4 ORNL LOANEES

R. W. Morrow, a graduate student in the Department of Chemistry with Professor J. A. Dean at the University of Tennessee, Knoxville, is conducting research toward the Ph.D. degree. In the Analytical Methodology Group with W. D. Shults and M. R. Guerin, he is studying flame-emission and atomic-absorption techniques as gas chromato- graphic detectors and numerous uses of these specific detectors in the gas chromatography of silicon derivatives. L. P. Turner 111, a Visiting Professor from the Department of Chemistry, University of Tennessee, Knoxville, continued the pyrolytic gas chromatography of macromolecules with A. S. Meyer, Reactor Projects Group. He has submitted an article on this work for publication. F. L. Whiting, a graduate student in the Department of Chemistry with Professor Gleb Mamantov at the University of Tennessee, Knoxville, is continuing his doctoral thesis research. In the Reactor Projects Group with J. C. White and J. P. Young, he is studying the simultaneous electrochemical generation and absorption spectro- photometric identification and characterization of solute ions of unusual oxidation states in molten fluoride melts (Sect. 3.2.i). J. C. Wolford, a first-year graduate student in the Department of Chemistry with Professor J. A. Dean at the University of Tennessee, Knoxville, is doing his doctoral thesis research in the Analytical Biochemistry Group with Gerald Goldstein. He is studying the separation of compounds of biological interest by ligand-exchange chromatography.

14.5 SUMMER STUDENT PROGRAMS

In the summer of 1968, five students participated in summer student programs.

14.5.a ORAU Student Trainee Program Linda J. Crist, now a senior at Arkansas State University, Jonesboro, worked withHelen P. Ruuen, Methodology Group, to investigate the thin-layer chromatography of steroids (Sect. 2.2.e) and the application of mass spectrometry (Sect. 2.2.0 and infrared spectrometry (Sect. 2.2.g) to the identification and measurement of steroids so isolated. 10 1

Marcia A. Lepri, now a senior at Mount Holyoke College, South Hadley, Mass., worked in the Nuclear and Radiochemical Group with W. S. Lyon on the decay scheme of ' Pd-' Rh (Sect. 8.3.e) and withJ. F. Emery on a number of special activation-analysis problems including the calibration of Ge(Li) detectors (Sect. 8.3.0. I D. R. Martin, now a senior at Sacramento State College, Sacramento, Calif., worked with W. L. MQ~~OXand D. J. Fisher, Analytical Instrumentation Group, to examine the performance of D.M.E.'s with a digital instrument computer and to explore the utilities of digital data acquisition and ensemble averaging in polarography (Sect. 1.21).

14.5.b ORNL Undergraduate Program

J. D. Lodmell, a graduate of Concord College, Athens, W.Va., now a first-year graduate student at the University of Tennessee, Knoxville, worked with the Reactor Projects Group. With A. D. Horton he performed special gas-chromatographic analyses and used gas chromatography as a preparative technique (Sect. 2.1.g). With R. F. AppZe and A. S. Meyer he assisted in the development of analytical methods for radioactive fluoride salts (Sects. 3.1.b and 3.l.c). F. V. Newsome, a graduate of Harvard University, Cambridge, Mass., now a first-year student at the University of West Virginia Medical School, Morgantown, worked with 1. B. Rubin, Analytical Biochemistry Group. He assisted in the development of an isotope-dilution technique for the determination of amino acids.

14.6 ALIEN GUESTS IN RESIDENCY

One scientist from another country is now a guest in the Analytical Chemistry Division.

Guest Sponsor Division Group

Young Kuk Kim International Atomic Energy Agency Nuclear and Radiochemistry Group Atomic Energy Research Institute Chyungryang-ri Sequl, Korea

i Part E. Ex t r a1 ab or at ory Professional Activities

The extralaboratory professional activities of members of the Division are numerous and varied. They reflect participation in a diversity of work, especially at the national and international levels.

W. L. Belew W. L. Belew is on temporary assignment to the Analytical Chemistry Group at the Australian Atomic Energy Commission Research Establishment at Lucas Heights, N.S.W., Australia 2232, under the USAEClAAEC exchange of technical personnel. At the Second Australian Conference on Electrochemistry, [Jniversity of Melbourne, February 19-23, 1968, he presented a paper on an ORNL cell design for minimizing iR error in controlled-potential polarography. He has assisted in the check-out of the ORNL model Q-2792 polarograph and the model Q-2942 D.M.E. droptime controller fabricated there and has demonstrated the satisfactory performance of these instruments compared with that of the Davis A-1660 polarograph. Now he is doing electroanalytical research with T. M. Florence under the direction of Dr. Lloyd Smythe (Sects. 1.7 and 1.11).

A. E. Cameron Member: International Commission on Atomic Weights International Union of Pure and Applied Chemistry (IWAC) Advisory Board (1 967-1 969) Analytical Chemistry

L. T. Corbin Member: Subcommittee N5.1, Fuel Manufacture and Fabrication American Standards Association (ASA) ASTM Committee E-IO on Radioisotopes and Radiation Effects ASTM Committee E-21 on Fuel Fabrication

J. M. Dale Chairman: General Session Analytical Chemistry Division 155th National American Chemical Society Meeting San Francisco. California Secretary-Treasurer: Analytical Group East Tennessee Section American Chemical Society

102 103

J. S. Eldridge Secretary: Subcommittee on the Use of Radioactivity Standards Committee on Nuclear Sciences National Academy of Sciences-National Research Council (NAS-NRC)

C. Feldman Chairman: Task Group on Photographic Photometry Committee E-2 on Emission Spectroscopy American Society for Testing and Materials (ASTM) Member: Editorial Board Optics and Spectroscopy

D. J. Fisher Member: Editorial Board Chemical Instrumentation

A. D. Horton Member: Subcommittee 111, Research ASTM Committee E-19 on Chromatography

C. A. Horton C. A. Horton is spending a second year at the Seibersdorf Laboratory of the International Atomic Energy Agency, Vienna, Austria. He is there as head of the analytical chemistry work.

M. T. Kelley Member: Chemistry Directors’ Meeting Division of Research United States Atomic Energy Commission Washington, D.C. Analytical Specialists Group Technology Subcommittee Union Carbide Corporation Member: Program Review Committee Chemistry Section Laboratory of Nuclear Science Massachusetts Institute of Technology Committee on Analytical Chemistry (1966-1969) Division of Chemistry and Chemical Technology National Academy of Sciences-National Research Council (NAS-NRC) Advisory Commit tee Microchemical Journal Board of Editorial Advisors Analytica Chimica Acta 1

104

C. E. Lamb Member: Executive Committee (1967-1970) Remote Systems Technology Division American Nuclear Society (ANS) Chairman: Membership Committee (1967-1968) (Also of ANS Remote Systems Technology Division)

W. S. Lyon Liaison Officer: ASTM Committee E-10 on Radioisotopes and Radiation Effects Member: Subcommittee I, Burnup ASTM Committee E-10 Subcommittee 111, Tracer Applications (Also of Committee E-10) Subcommittee V, Neutron Dosimetry (Also of Committee E-10) Editorial Board Chemical Instrumentation

Scientific Committee 25 OR Radiation Protection in the Use of Small Neutron Generators National Council on Radiation Protection and Measurement I Committee N43-3, Equipment for Non-Medical Radiation Applications United States of America Standards Institute Chairman: Referee Committee F, Industrial Wastes Subcommittee on Radiological Methods for Biological and Environmental Samples American Public Health Association (APHA)

T. R. Mueller Session Chairman: 21st Annual Summer Symposium “Computer Assisted Analytical Chemistry” The Pennsylvania State University, June 19-21, 1968

S. A. Reynolds Vice-chairman: Subcommittee .4, Methods of Radiochemical Analysis ASTM Committee D-19 Member: ASTM Committee D-19 on Water ASTM Committee E-10 on Radioisotopes and Radiation Effects Subcommittee 111, Tracer Applications ASTM Committee E-10 Task Group on Neutron Cross Sections (Also of Committee E-10)

I

3 105 n Task Group on Nuclear Data and Radiation Safety (E-10) Subcommittee on Use of Radioactivity Standards, National Research Council Task Group 1 of Scientific Committee 18 (Standards) of National Council on Radiation Protection and Measurements (NCW Member: Subcommittee on Radiological Methods for Biological and Environmental Samples American Public Health Association (APHA)

E. Ricci Member: Executive Committee Radiations and Isotopes Division American Nuclear Society (ANS)

W. D. Shults Member: Program Committee Analytical Group East Tennessee Section American Chemical Society Committee E-19 (Chromatography) American Society for Testing and Materials

P. F. Thomason Participant: Cloud Gap34 Project, October 16-23, 1967

J. C. White Secretary-Treasurer : Division of Analytical Chemistry (1967-1969) American Chemical Society (ACS)

Representative from the ACS to: Project N1 1, Basic Materials and Materials Testing for Nuclear Applications Nuclear Standards Board United States of America Standards Institute (Sponsored by ASTM) Member: Editorial Board A nalytical Letters Standing Committee for Sodium Impurities New York Operations Office United States Atomic Energy Commission Committee on Analytical Chemistry National Academy of Sciences-National Research Council (NAS-NRC)

A Chairman: Subcommittee on Reference Materials NAS-NRC Committee on Analytical Chemistry Presentation of Research Results

Several of the presentations listed below are made jointly with members of other divisions. In these cases the member(s) of the other division(s) is indicated by a single asterisk.

Publications

BOOK

AUTHORS TITLE PUBLISHER 1 Raaen, V. F.,* Carbon-I4 McCraw-Hill, G. A. Ropp,’ New York, 1968 Helen P. Raaen CONTRIBUTIONS TO BOOKS

AUTHOR(S) TITLE PUBLISHER 2 Bate, L. C., “Forensic Application of Trace Elements in Hair,” Gulf General F. F. Dyer pp. 247-259 in Proceedings of the First Atomic, Inc., International Conference on Forensic Activation San Diego, AmIysis held September 19-21, 1966, in San Calif. Diego, Calif. (V. P. Guinn, ed.), GA-8171 (1967) 3 Goldstein, G., “A Semi-Automated Filter Paper Disk Technique for Mediad, New York, W. L. Maddox, the Determination of Transfer Ribonucleic Acid,” 1968 I. B. Rubin pp. 47-49 in Technicon Symposia 1967, Automution in Analytical Chemistry, New York, October 2-4, 1967 4 Lyon,W.S. “Physical Techniques of Activation,” pp. 13-30 International Atomic in Nuclear Activation Techniques in the Life Energy Agency, Sciences (Proceedings of the Symposium Vienna, 1967 on Nuclear Activation Techniques in the Life Sciences, IAEA, Amsterdam, May 8-12, 1967)

THESIS

AUTHOR TITLE PUBLISHER 5 Lyon,W.S. Validity of Some Tests of Intellectual Ability University of for Predicting Grades in Related Craft Training Tennessee, Knoxville, (M.S. thesis) August 1968

‘Professor of Chemistry, Coker College, HartsviUe, S.C.

106 107

A ARTICLES

AUTHOR(S) TITLE PUBLISHER 6 Bamberger, C. E.,* “Containment of Molten Fluorides in Silica. Part I. J. Inorg. Nucl. Chem. J. P. Young, Effects of Temperatures on the Spectrum of fl 30, 1979 (1968) C. F. Baes, Jr.* in Molten BeFz-LiF Mixtures’’ 7 Bate, L. C., “Particle Size Distribution of Particles from 10 Anal. Chem. 40,468 F. F. Dyer to 2000 Microns by Sedimentation Analysis” (1968) 8 Bell, J. T.,* “Absorption of the Uranyl Ion in Perchlorate Media. J. Mol. Spectry. 25, R. E. Biggers2 111. Resolution of the Ultraviolet Band 312 (1968) Structure; Some Conclusions Concerning the Excited State of U02H.1r 9 Burtis, C. A., “Terminal Nucleoside Assay of Ribonucleic Acid Anal. Biochem. 23,502 G. Goldstein by Ligand-Exchange Chromatography” (1968) 10 Burtis, C. A., “Identification of UMary Constituents Isolated Clin Chem. 14,290 K. S. Warren* by Anion Exchange Chromatography” (1968) 11 Dyer, F. F., “A Film Recording Radiation-Event Monitor for Nucl. Instr. Methods L. C. Bate, Pulsed X and Gamma Radiation” 58, 157 (1968) L. H. Thacker* 12 Dyer, F. F., “ThreeDimensionally Rotating Sample Holder for Anal. Chem. 39,1907 L. C. Bate, 14-Million Electron Volt Neutron Irradiations” (1967) J. E. Strain 13 Farrar, L. G., “Chromatographic-Solvent Extraction Isolation of Anal. Chem. 40,1602 J. H. Cooper, Berkelium-249 from Highly Radioactive Solutions (1968) F. L. Moore and Its Determination by Beta Counting” 14 Hahn, R. L.* “The Recoil Technique and Its Possible Use in Anal. Chem. 40,219 Activation Analysis” (1968) 15 Hahn, R. L.,* “Interactions of 3He Particles with B, N, Nucl. Phys. AlOl, 353 E. Ricci Na and Be” (1967) 16 Hertel, G. R. “Surface Ionization. 111. The First Ionization J. Chem. Phys. 48, Potentials of the Lanthanides” 2053 (1968) 17 Hupf, H. B.,* “Production of Iodine123 for Medical Intern .IAppl. J. S. Eldridge, Applications” Radiation Isotopes J. E. Beaver* 19,345 (1968) 18 Kubota,H. “Rapid Distillation Separation of Microgram Microchem. J. 12, Quantities of Fluoride” 525 (1967) 19 “Chlorine Production by Gamma Radiolysis of Acid Anal. Chem. 40,271 Chloride Solutions and Its Effect on Analytical (1968) Procedures” 20 Lyon, W. S., “Nucleonics” Anal. Chem. 40(5), E. Ricci, 168R (1968) H. H. Ross 21 Maddox, W. L., “An Automatic Sampler for Obtaining Discrete Chem. Instr. 1,105 M. T. Kelley Samples from the Output of a Continuous-Flow (1968) Analyzer’’ 22 Mamantov, G.,3 “Electrochemical Reduction of U(1V) in Molten J. Electroanal. Chem. D. L. Manning LiF-BeFz-ZrF4 (65.6-29.4-5.0 mole %). 18,309 (1968) Evidence for Adsorption of U(1V)” 23 Manning,D. L. “Disproportionation of Electrochemically- J. Electroanal. Chem. G. Mamantov 1 Generated Uranium(V) in Molten LiF-BeFz-ZrF4 18,137 (1968) at SOO’C“

2Present address: Coca Cola Research Laboratory, Atlanta, Ga 3Consultant; Associate Professor of Chemistry, University of Tennessee, Knoxville. 108

24 Moore, F. L. “New Method for the Rapid Separation of Anal Chem. 39,1874 Berkelium(1V) from Cerium(1V) by Anion (1967) Exchange” 25 Mueller, T. R. “On the Separation of Half-Wave Potentials Chem. Instr. 1,113 Required for Resolution of Simple, Reversible, (1968) Overlapping Waves in Stationary Electrode Voltammetry” 26 Potterton, “An Evaluation of the Performance of the Nitrate- Anal. Letters 1, 1 1 Susan s.,“ Selective Electrode” (1967) W. D. Shults 27 Raaen, Helen P., “Resolution of Complex Mixtures of Nucleic Acid J. Chromatog. 35,531 Frances E. Bases, Nucleosides, and Nucleotides by Two- (1968) Krauss Dimensional Thin-Layer Chromatography on Polyethyleneimine-Cellulose” 28 Reynolds, S. A. “Availability of Standards for Common Isotopes Radiation Radionuclides” Technol. 5,118 (1968)

29 Reynolds, S. A., “Half-Lives of Radionuclides - 111” Nucl. Sci. Eng. 32, J. F. Emery, 46 (1968) E. 1. Wyatt 30 Ricci, E., “Rapid Calculation of Sensitivities, Interferences, Anal. Chem. 40,54 R. L. Hahn* and Optimum Bombarding Energies in 3He (1968) Activation Analysis” 31 Ross, H. H. “Analytical Applications of the Secondary Effects Record Chem. Progr. 28, of Radiation: Precision Photometry Using a 261 (1967) Radioisotopic Light Source’’ 32 Shults, W. D., “Synopsis of Eleventh Conference on Analytical Anal. Chem. 40(3), H. H. Ross, Chemistry in Nuclear Technology” 71A (1968) E. Ricci 33 Shults, W. D., “Controlled-Potential Differential DC Chem. Instr. 1, I D. J. Fisher, Polarography. V. Subtractive Polarography” (1968) W. B. Schaap6 34 White, J. C. “Standard Reference Materials as Viewed by the Anal. Chem. 40(3), (Chairman), Laboratory Supervisor - A Status Report” 24A (1968) M. D. C~oper,~ H. Fi~chbach,~ C. Merrit, JI.,~ G. H. Mor~ison,~ A. tho ma^,^ S. M. T~thill,~ S. vigo7 35 White, J. C. Book Review of: Analytical Chemistry of Anal. Chem. 40(1), Plutonium, P. N. Palei, ed., Daniel Davey & Co., 96A (1968) New York, 1967 36 Zittel, H. E., “A Voltammetric Method for Fluoride” Anal. Chirn. Acta 40,27 T. M. Florence’ (1968)

40RAU Student Trainee from Randolph-Macon Woman’s College, Lynchburg, Va.; summer 1967. ’ORAU Student Trainee from Nazareth College, Nazareth, Ky.; summer 1967. 6Professor of Chemistry, Indiana University, Bloomington. 7Member of the Subcommittee on Reference Materials, Committee on Analytical Chemistry, Division of Chemistry and Chemical Technology, National Academy of Sciences-National Research Council. 8Alien guest from Australian Atomic Energy Commission, Sutherland, New South Wales, Australia. 109

n REPORTS

REPORT NO. TITLE AUTHOR(S) AND DATE

37 Butts, W. C. Catalog of Gas Chromatographic Retention Data ORNL-TM-2374 (May 13, for Urinary Constituents and Related Compounds 1968) 38 Guyon, J. C.,9 Spectrophotometric Determination of Total ORNL-TM-2108 J. R. Stokely, Plutonium: Observations on the Reactions (Jan. 2, 1968) W. D. Shults Between Arsenazo and Pu(llI), Pu(IV) and Pu( VI) 39 Kelley, M. T. Statistical Quality Control Report, Analytical Oct. 20, 1967 Chemistry Division, July Through September 1967 (unpublished) 40 Statistical Quality Control R eport, Analytical Jan. 12, 1968 Chemistry Division, October Through December I96 7 (unpublished) 41 Statistical Quality Control Report, Analytical Apr. 18, 1968 Chemistry Division, January Through March 1968 (unpublished) 42 Statistical Quality Control Report, Analytical Oct. 14, 1968 Chemistry Division, April Through June I968 (unpublished) 43 Report of Foreign Travel to Czechoslovakia, Dec. 7, 1967 Yugoslavia,Austria, Greece, August 29, I96 7, (unpublished) Through October 8, 196 7 44 Report of Foreign Travel to Australia, February I, May 7, 1968 1968, Through March 7, 1968 (unpublished) 45 Lupica, S. B. Liquid Scintillation Counting of Weak Beta Jan. 8,1968 Emitters in Aqueous Solution Using Triton X-100 (unpublished) 46 Macklin, R. L.,* Proton Reaction Analysis for Lithium and Fluorine ORNL-TM-2238 J. H. Gibbons,* in Graphite, Using a Slit Scanning Technique (July 1968) T. H. Handley 47 Meyer, A. S., Jr. Report of Foreign Travel to Czechoslovakia,Italy, Nov. 2, 1967 Switzerland, Germany, West Germany, Norway, and (unpublished) England, September 2, 1967, Through September 30, 1967 48 Mueller, T. R., Modification of the ORNL Model Q-2564 High- ORNL-TM-2 175 H. C. Jones, Sensitivity Coulometric Titrator (Mar. 18,1968) D. J. Fisher, R. W. Stelzner 49 Raaen, Helen P., ed. Analytical Chemistry Division Annual Progress ORNL-4196 Report for Period Ending October 31, 1967 (January 1968) 50 Raaen, Helen P., Cumulative Indexes to the Analytical Chemistry ORNL-3904, rev. 2 Ann S. Klein,* eds. Division Annual Progress Reports 1964-1 96 7 (January 1968) 51 Reed, R. E.,* Sources of Contamination During Electron-Beam ORNL-TM-2208 C. W. Dean,* Melting (July 1968) R. E. McDonald,* J. F. Emery 52 Ricci. E. Report of Foreign Travel to France, Italy, Nov. 2, 1967 Germany, The Netherlands, and Harwell, England, (unpublished) September 5, 1967, Through September 26, 1967 53 Strain, J. E., The Design and Evaluation of a Delayed-Neutron ORNL-4 135 W. J. Ross, Leached-Hull Monitor (February 1968) G. A. West,* J. W. Landry*

(19 90RAU Research Participant; Associate Professor of Chemistry, University of Missouri, Columbia. 110

54 White, J. C. Analytical Chemistry Research and Development Nov. 29, 1967 Monthly Summary - November 1967 (unpublished) 55 Analytical Chemistry Research and Development Jan. 4, 1968 Monthly Summary - December I967 (unpublished) 56 Analytical Chemistiy Research and Development Jan. 26, 1968 Monthly Summary - January I968 (unpubhshed) 57 Analytical Chemistry Research and Development Feb. 28, 1968 Monthly Summary - February 1968 (unpublished) 58 Analytical Chemistry Research and Development Mar. 26, 1968 Monthly Summary - March 1968 (unpublished) 59 Analytical Chemistry Research and Development Apr. 29, 1968 Monthly Summary - April I968 (unpublished) 60 Analytical Chemistry Research and Development May 29, 1968 Monthly Summary - May 1968 (unpublished) 61 Analytical Chemistry Research and Development June 28, 1968 Monthly Summary - June I968 (unpublished) 62 Analytical Chemistry Research and Development July 26, 1968 Monthly Summary - July I968 (unpublished) 63 Analytical Chemistry Research and Development Aug. 28, 1968 Monthly Summary - August 1968 (unpublished) 64 Analytical Chemistry Research and Development Sept. 30, 1968 Monthly Summary - September 1968 (unpublished) 65 Zittel, H. E. Report of Foreign Travel to England, Switzerland, Aug. 23, 1968 Italy, Germany, and The Netherlands,July IO, 1968, (unpublished) Through July 31, 1968 66 Anonymous “Polarographic Drop Time Controller/Q-2942/” in CAPE-165 1 Engineering Materials List, TID4100 67 “Controlled-Potential D. C. Polarograph- CAPE-1652 Voltammeter/Q-2792” in Engineering Materials List, TID-4100 68 “Controlled-Potential and Controlled-Current Cyclic CAPE-165 3 Voltammeter” in Engineering Materials List, TID4100 69 “Automatic Potentiometric Titrator” in CAPE-368 (revised) Engineering Materials List, TID4100 70 “High-Sensitivity Coulometric Titrator/Q-2564/” in CAPE-1 196 (revised) Engineering Materials List, TID-4100 71 “ServeControlled Pipetters” in Engineering CAPE-1220 (revised) Materials List, TID-4100

METHODS ISSUED TO THE ORNL MASTER ANAL YTICAL MANUAL

New Methods

FORMAL ISSUES

AUTHOR TITLE NUMBER DATE , 72 Mueller, T. R. “Cyclic Voltammeter, 1003045 9-1-68 Controlled-Potential, 9 003045 Con trolled-Current” 73 Maddox, W. L. “Filter Photometers, 1003092 3-1-68 Remotely Operated, 9 003092 ORNL Models 91734 and 64-3171” 111

74 Wyatt, E. I. “Strontium-92, Product 9 0733805 1-27-67 Analysis Guide” 75 “Strontium-90, Product 9 0733806 1-27-67 Analysis Guide”

RECORDCOPY ISSUES

AUTHORS TITLE NUMBER DATE 76 Crist, Linda J.,” “Separation of Six 100714 8-12-68 Helen P. Raaen Corticosteroids by Thin- Layer Chromatography on Gelman ITLC-SA Medium”

Revised Methods

AUTHOR(S) TITLE NUMBER DATE 77 Jones, H. C. “Coulometric Titrator, 1003025 R.3-1-68 Controlled-Potential, 9 003025 High-Sensitivity, ORNL Model Q-2564” 78 Wagner, E. B., “Automatic Potentiometric 1003028 R.3-15-68 W. L. Maddox Titrator, Velocity-Servo, 9 003028 ORNL Models Q-1728 and Q-1728A” 79 Wyatt, E. I. “Proportional Beta Counter, 2 00352 R.3-1-68 Windowless” 5 00352 9 00352 80 Rickard, R. R. “ Radioactivity in 2 21734 R.3-15-68 Aqueous Solutions, 9 062310 Pyridine Extraction-Gamma Counting Method” 81 Apple, R. F. “Fluoride in MSRE Fuel, 9 021203 R.3-1-68 Pyrolysis Method” 82 McDowell, Betty L., “Niobium in Mixtures of 9 0922550 R.3-15-68 D. C. Canada Fluoride Salts, Spectro- photometric Thiocyanate Method“

Oral Presentations

AT MEETINGS OF PROFESSIONAL SOCIETIES, CONFERENCES, AND THE LIKE AUTHOR(S) TITLE PRESENTEDAT

83 Belew, W. L.,l “A Cell Design for Minimizing iR Error in Controlled- Second Australian Conference on Electrochemistry, D. J. Fisher, Potential Polarography” Royal Australian Chemical Institute, Melbourne, M. T. Kelley, Australia, Feb. 19-23, 1968 J. A. Dean’

~ “ORAU Student Trainee from Arkansas State University, Jonesboro. ‘Speaker. “Consultant; Professor of Chemistry, University of Tennessee, Knoxville. 112

84 Burtis, C. A. “Fractionation of Human Urine by Gel Annual Meeting, American Association of Clinical Q Chromatography” Chemists, Washington, D.C., Aug. 9-23, 1968 85 Burtis, C. A.,’ ’ “Assay of 3’-Terminal Nucleosides of Transfer Southeastern Regional Meeting, American G. Goldstein Ribonucleic Acids by Ligand Exchange Chemical Society, Atlanta, Ga., Nov. 1-3, Chromatography” 1967 86 Burtis, C. A.,’ ’ “Identification of Urinary Constituents Isolated Symposium on Urinary Constituents of Low K. S. Warren* by Anion-Exchange Chromatography” Molecular Weight, Oak Ridge National Laboratory, Oak Ridge, Tenn., Nov. 30-Dec. 1, 1967 87 Dale, J. M.,” “A Transpiration Method for the Determination of 155th Meeting, American Chemical Society, R. F. Apple, U(II1) in Radioactive Molten Salt Reactor Fuel” San Francisco, Calif., Mar. 3 1-Apr. 5, 1968 A. S. Meyer 88 Dean, C. W.,* ’ ’ “Sources of Contamination During Electron Beam Third International Conference on Electron and R. E. Melting” Ion Beam Science and Technology, Boston, McDonald,* Mass., May 6-9, 1968 R. E. Reed,* J. F. Emery 89 Feldman, C. “Beam-Splitter for Use in Calibrating Spectrographic 7th National Meeting, Society for Applied Emulsions” Spectroscopy, Chicago, Ill., May 13-17, 1968 90 Kelley, M. T. “What Industry Expects of the Graduate in 19th Southeastern Regional Meeting, American Chemistry or Chemical Engineering” Chemical Society, Atlanta, Ga, Nov. 1-3, 1967 91 “Some Approaches to More Rapid Analysis” 1967 Eastern Analytical Symposium, New York, Nov. 8-10, 1967 92 “Analysis for Nuclear Reactors” Seminar, AAEC Research Establishment, Lucas Heights, New South Wales, Australia, Feb. IS, 1968 93 “Electroanalytical Research at Oak Ridge National Seminar, University of New South Wales, Sydney, Laboratory” Australia, Feb. 16, 1968 94 “Electronic Instrumentation” Second Australian Conference on Electrochemistry, (Invited Lecture) Royal Australian Chemical Institute, Melbourne, Victoria, Australia, Feb. 21, 1968 95 “Electroanalytical Research at Oak Ridge National Analytical Chemistry Group, Perth, Australia, Laboratory” Feb. 23, 1968 96 “Electroanalytical Research at Oak Ridge National Analytical Chemistry Group, Adelaide, Australia, Laboratory” Feb. 26, 1968 97 “The Analytical Chemistry of the Actinide Elements” Royal Australian Chemical Institute, Canberra, (Invited Paper) Australia, Feb. 28, 1968 98 “Electroanalytical Research at Oak Ridge National Analytical Chemistry Group, Brisbane, Australia, Laboratory” Mar. 1, 1968 99 “The Analytical Chemistry of the Actinide Elements” Royal Australian Chemical Institute, Newcastle, (Invited Paper) Australia, Mar. 4, 1968 100 “The Role of the Large National Research Royal Australian Chemical Institute, University Laboratories in the USA” of New South Wales, Australia, Mar. 6, 1968 101 “Operational Amplifier Systems in Electroanalytical Central Regional Meeting, American Chemical Chemistry at.Oak Ridge National Laboratory” Society, Akron, Ohio, May 9-10,1968 (Invited Paper) 102 “A Comparison of Methods of Analytical Chemistry” ORAU Neutron Activation Course, Special Training Division, Oak Ridge, Tenn., Aug. 12-30, 1968 . 103 Kubota, H. “Homogeneous Precipitations Using Radiolytically 155th Meeting, American Chemical Society, Generated Hydrochloric Acid” San Francisco, Calif., Mar. 31-Apr. 5, 1968

104 Lyon, W. S. “Prospects and Problems for Activation Analysis of D.I.D. Roundtable on Development of Nuclear Ocean Sediments” Techniques for Rapid Analysis of Ocean Elements, A Washington, D.C., Oct. 16, 1967 113 n

105 “Activation Analysis Interferences” ORAU Neutron Activation Analysis Course, Special Training Division, Oak Ridge, Tenn., Aug. 28, 1968 106 “Recent Advances in Activation Analysis” Midwest Regional Meeting, American Chemical Society, Columbia, Mo., Nov. 2-3, 1967 107 “Basic Concepts of Activation Analysis” Radioisotopes in Medicine in Vitro Studies, ORAU, Oak Ridge, Tenn., Nov. 13-16, 1967 108 Manning, D. L., “Electro-reduction of Uranium(1V) in Molten Second Australian Electrochemistry Conference M. T. Kelley,’ ’ Lithium FluorideBeryllium Fluoride-Zirconium of Royal Australian Chemical Institute, G. Mamantov3 Fluoride at Fast Scan Rates and Short Transition Melbourne, Australia, Feb. 21, 1968 Times” 109 Manning, “Disproportionation of Electrochemically Generated 155th Meeting, American Chemical Society, D. L.,” Uranium(V) in Molten LiF-BeFz-ZrF4 at San Francisco, Calif., Mar. 31-Apr. 4, 1968 G. Mamantov3 50O0C’ 110 Manning, “Voltammetric Studies of Cr(I1) in Molten Lithium 156th Meeting, American Chemical Society, D. L.,’ ’ Fluoride-Beryllium Fluoride-Zirconium Fluoride at Atlantic City, N.J., Sept. 8-13, 1968 J. M. Dale 50O0C’ 111 Ricci, E. “Experience and Future Outlook on He-Activation National Bureau of Standards, Washington, D.C., Analysis” (Invited Lecture) Oct 23, 1967

112 “Activation Analysis with 25 ’Cf Neutrons” ORNL Transuranium Research Laboratory, Oak Ridge, Tenn., Jan. 11, 1968 (Lecture to visiting ORAU Group) 113 Ricci, E.,” “Neutron Activation Analysis with ”’Cf Sources” Transplutonium Program Committee Meeting. The T. H. Handley Transplutonium Elements: Availability and Applications, AEC Headquarters, Germantown, Md, Apr. 18, 1968 114 Ricci, E. “New Developments in Activation Analysis” (in Argentinian Atomic Energy Commission, Buenos Spanish) Aires, Argentina, July 29, 1968 115 Roche, “Investigation of 7-Rays in the Decay Chain Spring Meeting, American Physical Society, M. F.,*” 1 72Hf+ 1 72Lu + 172yr> Washington, D.C., Apr. 22-25, 1968 K. S. Toth,* R. L. Hahn,* C. R. Bemis,* T. H. Handley

116 Ross, H. H. “Nuclear Methods for Extra Terrestrial Analysis” ORAU Special Seminar, ORAU, Oak Ridge, Tenn., Jan. 9, 1968 117 “Theory and Practice of Liquid Scintillation Isotope Technology Training Course, ORAU, Counting” Apr. 23, 1968 118 “Modern Nuclear Instrumentation” ORAU Special Seminar, ORAU, Oak Ridge, Tenn., July 31, 1968 119 Shults, W. D. “Recent Advances in Differential Polarography” University of Georgia, Athens, Mar. 14, 1968 120 “Performance Characteristics of Ion-Selective Union Carbide Corporation Analytical Specialist Electrodes” Meeting, Bound Brook, N.J., May 20, 1968 121 Strain,J.E. “Standard Gamma-Ray Spectra of the Elements Conference, Small Accelerators for Teaching and Following 14-MeV Neutron Irradiations” Research, Oak Ridge Associated Universities, Oak Ridge, Tenn., Apr. 8-10, 1968 122 White, J. C. “Analytical Chemistry” Engineering Training Seminar, Oak Ridge National Laboratory, Oak Ridge, Tenn., Mar. 15, 1968 123 Young, J. P. “Absorption Spectra of Several Transition Metal Ions 155th Meeting, American Chemical Society, in Molten Fluoride Solution” San Francisco, Calif., Mar. 31-Apr. 5, 1968 124 “Spectrophotometric Studies of Solute Species in 156th Meeting, American Chemical Society, Molten Fluoride Media” (Invited Paper) Atlantic City, N.J., Sept. 8-13, 1968 125 Zittel, H. E.,’ ’ “Radiation and Thermal Stability of Sprays” American Nuclear Society Meeting, Toronto, T. H. Row* Canada, June 9-13,1968 126 Zittel, H. E. “The Effect of Radiation on Some Analytical Second Conference, Society for Analytical Methods” Chemistry, Nottingham, England, July 15-19, 1968 114

UNDER THE TRAVELING LECTURE PROGRAM

LECTURER TITLE PRESENTED AT 127 Cameron. A. E. “Geological Age Determination by Isotopic Indiana Central College, Measurements” Indianapolis, Nov. 28, 1967 128 “Geological Age Determination by Isotopic North Carolina State University, Measurements” Raleigh, Nov. 30, 1967 129 Ricci, E. “Recent Developments in Activation Analysis” Western Kentucky University, Bowling Green, Apr. 5, 1968

Patents

AUTHOR TITLE PATENT NO. DATE ISSUED 130 Moore, F. L. “Method for Separating Members of Actinide British Patent No. 1,098,350 Jan. 10, 1968 and Lanthanide Groups” Translations

ORIGINAL REFERENCE TRANSLATION Translator Author Translated ORNL-tr Source Language Language (Transliterated) Title Number

1 Kubota,H. K. Hamada, T. Hitachi Hyoron, Japanese English “Stress Analysis 1769 Hayashi, and 48,812-816, in Tapered Tran- I. Oguchi 1966 sition Joints in Reactor Pressure Vessel” 2 Kubota,H. T. Kamiyama Genshiryoku Japanese English “Trend in Atomic 1825 ~000,13(2), Power Generation 5-6, 1957 and Uranium Resources”

A

115 Articles Reviewed or Refereed for Periodicals

Number of Articles Reviewed or Refereed for Indicated Periodical

Reviewer or Referee

v, h .$v, c cu 4 0" .r' .i 4 E 4 T T

Bate, L. C. 1 1 1 Cameron, A. E. 1 Canada, D. C. 1 1 3 Dyer, F. F. 3 4 Emery, J. F. 4 6 Feldman, Cyrus 2 1 6 Fisher, D. J. 1 5 1 Goldberg, Gerald 1 6 Handley, T. H. 4 Horton, A. D. 1 1 8 Lyon, W. S. 3 1 4 Moore, F. L. 3 Mueller, T. R. 1 8 Reynolds, S. A. 1 2 1 2 Ricci, Enzo 6 Ross, H. H. 6 2 Ross, W. J. 2 2 Shults, W. D. 2 3 Stelzner, R. W. 3 Stokely, J. R. 1 1 4 White, J. C. 3 1 2 Young, J. P. 1 1 1 Zittel, H. E. -1 - Total 45 1 1 5 4 1 2 1 1 - __ -

116 Indexes

Helen P. Raaen Ann S. Klein'

Indexes are a part of the Analytical Chemistry Division annual report for the fifth time. The num- bering system used has made possible the preparation of cumulative indexes to the annual progress reports from -68 A-09-08 C the Division. This section of the report contains a key-word index and an author index to this report. The In the use of the index to locate material in the body of cumulative indexes for the years 1964-1968 are bound the report, only the last two groups of numbers are separately and are designated OWL-3904 (Rev. 3). needed, because the chapters are numbered consec- The Key Word Index is prepared both from the utively. numbered headings that appear within the report and For reference to the Presentation of Research Results, from the titles of the entries in the Presentation of the numbering system is of the type 68PRR-025, where Research Results and in the Translations sections. To 68 designates the year in which the entry was listed in increase the depth of indexing of the work reported, supplementary words were added to some of the the annual report, PRR identifies the authored work as being listed in the Presentation of Research Results part headings. These words appear in parentheses, together of the annual report, and 25 is the number of the entry with the heading, in the key-word index; they do not listed in that part of the report; for example, appear elsewhere in the report. The Author Index is an alphabetical listing of authors, YEIR Lv\ LISTED ENTRY together with number entries that specify the material I LISTED ENTRY IN THE INNUAL to which each author contributed. This index includes the authors of material in the body of the report, the authors of the entries listed in the Presentation of 68 P R R-025 Research Results, and the translators of the entries listed in Translations. In the cases of ceauthorships, the In the use of the Index to locate an entry in the member of another OWL division is so indicated by an Presentation of Research Results part of the report, asterisk which precedes that author's name. If, for any only the last group of numbers is needed, because the of a number of reasons, an author is not a permanent entries are numbered consecutively. member of OWL, the symbol = appears before his If the entry is in the Translations part of the report, name. the entry will be identified by the letters TR in the An example of the numbering system used to refer to same position as the letters PRR. material in the main body of the report is 68A-09-08C, Machine limitations necessitate that some entries be where 68 indicates the year of publication of the annual in an unusual form. Because special type cannot be report, A designates a major part or division of the used, entries that otherwise would require it are written report, 9 is the chapter number, 8 is a primary section out; for example, chemical symbols, chemical formulas, within the chapter, and C is a subsection (designated in Greek letters, 0-, m-,p, etc. Superscript and subscript the subsection heading with c instead of C); for numbers cannot be printed; hence, valence is designated example, by a Roman numeral following the name of the element or ion, and an isotope mass number is indicated by a 'Technical Information Division. hyphen and an Arabic number following the name of

117 118 the element. The lower-case m, used with an isotope Additional useful entries are provided by dividing mass number to designate a metastable state, appears as certain words; for example, ethylenediamine is divided a capital M in the listing. into ethylene, di, and amine. Chemical Titles is used as a guide in making such divisions. Key Word Index

AMANITA TOXINS IGALERINA MARGINATA I/ 68A-02-020 AININGl VALIDITY OF SOME TESTS OF INTELLFCTUAL ABILITY FCR PREDICTING GRADES IY REL4TFD CDAFT TR 6RPRR-GO5 STUDIES OF ABSOLUTE FILTERS/ 68A- 07-0 1B UMIIIII IN R DbCTIVE MIRE FUEL BY HYORIJGEN REOKTICN ( ABSORPTICN - THERMAL CONDUCTIVITY MEASUREMENT OF 68A-03-018 CONCLUSIONS UCERNING THE EXCITE0 STATF OF URANYL ION/ ABSORPTION OF THE URANYL ION IN PER CHLORATF MFOI 6ePRR-008 C 30 TRANSITION METAL IONS IN MOLTEN FLUORIDE SOLUTICN ( ABSORPTION SPECTRA OF IRON(II1t NICKELIIII~CHROM 68A-03-OZG NS IN MOLTEN FLUORIDE SOLUTION/ ABSORPTICN SPECTRA OF SEVERAL TRANSITION YFTEL IO 68PRR-123 OMIUM(I1 1, AND CFROMIUMI I111 IN MOLTEN FLUORIDE SALTS I/ ABSORPTICh SPECTRA OF SEVERAL 30 TRANSITION MFTbL 68b-C3-02G TER I AL S/ ABSORPTION SPECTROPHOTOMETRY OF ALPHA EMITTING MA 6RB-10-12 RON ACTIVATION 4NALYSIS AT THE OAK RIDGE ELECTRCN LINEAR ACCELERATCR I ORELA I/ PHOTON AUD FAST NEUT aen-ce-ole TRNA I/ OETERMINATION OF METHIONINE ACCEPTING TRANSFFR RIBO NUCLFIC ACID ( METHIONINE 68b-04-018 RNA I/ OETERMINATION OF TYROSINE ACCEPTING TRANSFER RIEO NUCLEIC ACID I TYROSINF T 684-04-018 OR DESALTING AN0 REMOVING ORGANIC COMPOUNDS FROM WATER ( ACETATE / AMRERLITE XAO-2 I/ EVALUATION OF A LTPrl 68A-02-058 NO ACTINIDES I AMERICIUM / EUROPIUM / HEX4 FLUORO ACETYL ACETONE / Z,Zt6r6 TETRA METHYL 3.5 HEPTINE DIONE 68A-02-07G POLAROGRAPHY OF ZIRCONIUM IN ACETONITRILE PNO CI METHYL SULfOXIDEl 68A-01-07 NIOES AN0 ACTINIDES I AMERICIUL / EUROPIUM / HEYA FLUORC ACETYL ACETONE I 212r6,6 TETRA METHYL 315 HEPTANE 68A-02-076 RADIOLYSIS OF PER CHLORIC ACID/ 68A-OR-C7C Y OF SULFUR 01 OXIDE I SULFITE I IN AQUEOUS HYDROFLUORIC ACIOI POLAROGRAPH 68A-02-CBC ECIPITATIONS USING RAOIOLYTICALLY GENERATED HYDROCHLORIC ACID/ HOMOGENEOUS PR 6RPRR-103 TECHNIQUE'FOR THE OETERMINATION OF TRANSFER RIB@ NUCLEIC ACIOI A SEMIAUTCMATEO FILTER PAPER DISK 69PkR-CC3 L ALPHA RACIATION LABORATORY ( ALPHA HYDROXY IS0 BUTYRIC ACID I BERKELIUM-249 / CHROMATflGRAPHY / DISSOLUTI 088-12-01 E / TRUXENE / UREA / VARCUM / PAP1 / FURFURAL / HIPPURIC ACID / CARYOPHYLLENE / LIPIDS I/ NUCLEAR i4AGNETIC 6RR-11-04 ON I AS AN ACSORBENT ( 01 2 ETHYL HEXYL ORTHO PHOSPHORIC ACID / HOEHP / LIQIJIO ION EXCHANGERS I/ POLY TETR 684-02-028 NO ACIDS - CARBON-14 I CI 2 ETHYL HEXYL ORTHO PHOSPHORIC ACID / HOEHP / LIQUIO ION EXCHANGERS I/ RECLAIMIN 68A-04-01G ION I/ CONCENTRATING HYDROCHLORIC ACID I HYDROGEN CHLORIDE-36 / CONTROLLED OEHYORAT 686-02-050 ERMINATION OF METHIONINE ACCEPTING TRANSFER RIBO NUCLEIC ACID I METHIONINE TRNA I/ OE T 68A-04-018 GEL ELECTRCPHOQESIS OF RIBO NUCLEIC ACID I RNb I/ 68A-04-01J KINETICS OF AMINO ACYLATICN OF TRANSFER RIB0 NUCLEIC ACID I TRNA I/ h8 A- 04- C 1F ONOITIONS FOR THE DETERMINATION OF TRANSFER RIBO NUCLEIC ACID f TRNA I/ A FRACTIONPL FACTORIAL METHOD FOR 68A-04-01C LEIC ACID BASES I/ CONSTITUENTS OF TRANSFER RIBO NUCLEIC ACID I TRhA I I POLY ETHYLENE IMINE - CFLLULOSE / 68A-02-OZC ETERMINATION OF TYROSINE ACCEPTING TRANSFER RIB0 NUCLEIC ACID I TYROSINE TRNA I/ 0 68A-04-01A IMINE - CELLULOSE / NUCLEOSIDES / NUCLEOTIDES / NUCLEIC ACID BASES I/ CONSTITUENTS OF TRBNSFER RI90 NUCLE 68A-02-02C INE CELLULOSE/ RESOLUTION OF COMPLEX MIXTURES OF NUCLEIC ACID BASES, NUCLEOSIDES, AN0 NUCLEOTIDES 3Y TWO 0 6FPRR-027 TERMINAL NUCLEOSIDE ASSAY OF RIBO NUCLEIC ACID BY LIGANO EXCHANGE CHROMATOGRAPHY/ 68A-04-ClI TEQMINAL NUCLEOSIDE ASSAY OF RIBO NUCLEIC ACID BY LIGANO EXCHANGE CHROYATOGRAPHYI 68PRR-CC5 L PROCEDURES/ CHLORINE PRODUCTION BY GAMMA RADIOLYSIS OF ACID CHLORIDE SOLUTIONS AN0 ITS EFFECT ON 4NALYTI 68PRR-C19 AMINO ACID SEQUENCE OF MOUSE HEMOGLORINl 6BA-04-03H AMINO ACID SUBSTITUTIONS/ 686-04-031 E/ RAPID POLAROGRAPHY OF URANIUM IN 1 MOLAR HYDROFLUORIC ACID WITH A VERTICAL ORIFICE TFFLON DROPPING MEhC 68A-02-088 STABILITY OF SOME INERT METALS IN IRRADIATE0 MINERAL ACIDS/ 68A-OR-070 METHYL SILYL PHENYL THIO HYCANTOIN DERIVATIVES OF AMINO ACIDS I/ BIOMEOICPL PPPLICATIONS I FREE FATTY 4CI 088-02-010 Y NUCLEAR AROMATIC HYDROCARBONS, ALKALOIDS, PHENOLS, AN0 ACIDS I/ EXPLORATORY STUDIES I GAS CHROMATOGRAPHY 68A-02-03A ACID / HOEHP / LIQUIO ION EXCHANGERS I/ RECLAIMIhG AMINO ACIDS - CARBON-14 I CI 2 ETHYL HEXYL ORTHO PHOSPH 68A-04-01G S OF AMINO ACIDS I/ BIOMEOICAL APPLICATIONS I FREE FATTY ACIDS / AMINO ACIDS / PHENYL THIO HYOANTOIN OERIV 684-02-010 US I/ BIOMEDICAL APPLICATIONS I FREE FATTY 4CIDS I 4MINO 4CIDS I PHENYL THIO HYD4NTOIN DERIVATIVES OF AMIN 68A-02-CIlD TION FOR ANALYTICAL BIOCI-EMISTRY I TRANSFER RIB3 NUCLEIC ACIDS I TRANSFEP RNP / FILTER PAPER DISK TECHNIQU 68A-01-19 AMINO ACIDS / PHENYL TbIO HYOANTOIN DERIVATIVES OF AMINO ACIDS / TRI METHYL SILYL PHENYL THIO HYOANTOIN DE 68A-0 2-0 10 I DETERMINATION OF THE METHYL ESTERS OF BUTYL PHOSPHORIC ACIDS I TRI METHYL PHOSPHATE IO1 METHYL BUTYL PH 68A-02-01E AUTOMATED DETERHINbTION OF TRANSFER RIBO NUCLEIC ACIDS I TRNA I/ 68A-04-01D CHEMICAL ANALYSIS OF TRANSFER RIB0 NUCLEIC ACIDS I TRNA I/ 684-04-01H N COUNTING DATA IN THE ANALYSIS OF TRANSFER RI~O NUCLEIC ACIDS i TRNA 11 COMPUTER PROCESSING OF LIQUID SCI 68A-04-ClE OETERMINATION OF SUBNANDMPLE QUANTITIES OF L AMINO ACIDS BY ISOTOPE DILUTION - AMINO ACYLATION/ 68A-04-D1L SSAY OF 3/ TERMINAL NUCLEOSIDES OF TRANSFER RIBO NUCLEIC ACIDS BY LIGANO EXCHANGE CHROMATOGRAPHY/ A 48PRR-C85 METHOD FOR SEPARATING MEMBERS OF ACTINIDE AND LANTHANIDE GRQUPS/ 68PRR-130 THE ANALYTICAL CHEMISTRY OF THE ACTINIDE ELEMENTS/ 68PRR-097 D ANALYSIS OF THE BETA 01 KETONES OF THE LANTHANIDES AND ACTINIDES I AMERICIUM / EUROPIUM / HEXA FLUORO AC 68A-02-076 QUANTITATIVE ELECTRCOEPOSITION OF ACTINIDES FRLM 01 METHYL SULFOXIDE/ 6fA-Oe-020 PHYSICAL TECHNIQUES OF ACTIVATION/ 68PRR-004 ATOR STUDIES I OETERMINATION OF OXYGEN BY 14-HEV NEUTQON ACTIVATION I/ 14-MEV NEUTRON GFNER 63A-OR-05A ACTIVATION ANALYSIS/ 68A-08-0 1 INFLUENCE OF CbANhELING IN CUSTOMARY HELIUP-3 ACTIVATION ANPLYSISI 68A-Ce-ClO OETERMINATION OF FLUORINE IN FLUORSPAR BY 14-MEV NEUTRON ACTIV4TICh ANALYSIS1 68A-08-058 THE RECOIL TECbNIPUE AN0 ITS POSSIBLE USE IN ACTIVATICh ANALYSIS/ 68PRR-C14 RECENT ADVANCES IN ACTIVATION ANALYSIS/ 68PRR-106 BASIC CCNCEPTS OF ACTIVATION ANALYSIS1 68PRR-107 EXPERIENCE AN0 FUTURE OUTLOOK ON HELIUM-3 ACTIVATION ANALYSIS/ 68PRR-111 NEY DEVELOPMENTS IN ACTIVATION ANALYSIS/ 68PRR-114 RECENT DEVELOPMENTS IN ACTIVATION ANALYSIS/ 68PRR-129 TERFERENCES. AND OPTIMUM BOMBARDING ENERGIES IN HELIUM-3 ACTIVATION ANALYSIS/ RAP10 CALCULATION OF SENSITI 68PRR-030 EAR ACCELERATOR I DRELA I1 PHOTON AND FAST NEUTRON ACTIVATION ANALYSIS AT THE OAK RIDGE ELECTRON LIN 684-0 8-01 B ACTIVATION ANALYSIS INTERFERENCES1 68PRR-105 D MANGANESE1 NEUTRON KTIVATION ANALYSIS CF BRAIN TISSUE FOR COPPER AN 684-0 8-01F PROSPECTS AN0 PROBLEMS FOR ACTIVATION ANALYSIS OF OCEAN SEDIMENTS/ 68PRR-104 NEUTRON PCTIVATICN ANALYSIS WITH A CALIFORNIUM-252 SOURCE 68A-08-01C I ACTIVATION ANALYSIS WITH CAL I FOPN IUM-252 NEUTRONS 6BPRR-112 NEUTRON ACTIVATION ANALYSIS WITH CALIFORNIUM-252 SOURCFS/ 68PRR-113

119 QUANTITIFS OF L AMINO ACIOS BY ISOTOPF DILUTION - AMINO ACYLATION/ DETERMINATION OF SUBNANOMOLE 68 A- 04- 0 1L KINETICS OF AMINO ACYLATION OF TRANSFER RIB0 NUCLEIC ACID ( TRNA )I 68A-04-01F XCHANGERS )I POLY TETRA FLUORC ETHYLENE ( TEFLON l AS AN ADSORBENT ( DI 2 ETHYL HEXYL ORTHO PHOSPHORIC ACI 6 8A- 02- 026 IVY FLUORIDE ( 65.6-29."-5.0 MOLE PERCENT 1 EVIDENCE FOR ADSORPTION OF URAYIUM(IVI/ ELECTROCHEMICAL REOUCT 68PRR-022 PCFTATE / AMBERLITE XAO-2 )I EVALUATION OF A LIPOPHILIC ADSORPTION RESIN FOR DESALTING AND REMOVING ORGAN 684-02-058 RECENT ADVANCES IN ACTIVATION ANALYSIS/ 68PRR-106 RECENT ACVANCES IN DIFFERENTIAL POLAROGRAPHY/ 68PRR-119 / A CONTQOLLED POTENTIAL AN0 CERIVATIVF DC POLAROGRAPH - ADVANTAGES OF RAPID AND CIERIVATIVE OC POLAROGRAPH 686-01-06 ADVISORY COMMITTFE MEMBERS AND CONSULTANTS/ 680- 14- 0 1 GEOLOGICAL AGE DETERMINATIOY 8Y ISOTOPIC YEASUREMENTSI 68PRR-127 UTRON 1RPACIATION IN REMGTF FACILITIES DF UNEVEN FLUX/ AIR FLOATING SPHERE FOR HOMOCENFOUS PHOTON AN0 NF 68A-08-01A AIR QUALITY SURVEY/ baa-02-06 EHYDE / OPGLNO PkOSPhOQUS POLYMERS / 5 FURFbRYL FURFURYL ALCOHCL / OEUTERO CI METHYL SULFOXI@E / HEXA METH 688-11-04 VENE / POLY METHYLFNE POLY PHEYYL IS0 CYANATE / FURFURYL ALCOHOL / FURAN ALDEHYDE / OQGANO PHOSPHORUS POLY 688-11-04 YLENE POLY PHENYL IS0 CYANATE / FURFURYL ALCOHOL / FURAN ALDEHYDE / ORGAN0 PHOSPHORUS POLYMERS I 5 FURFURY 688-11-04 E I NITRATE / TECHNICON AUTCANALYZER / HYDROPONIC BEDS / ALGAL NUTRIENTS I/ EUTROPHIC WATER SYSTEMS ( PHOS 68A-02-048 ALIEN GUESTS IN KESIOFNCYl 680-14-06 AS CHRnMbTOGRAPHY OF POLY NUCLEAR AROMATIC HYDROCARBONSI ALKALOIDSI PHENOLS, AND ACIDS l/ EXPLORATOPY STUD baa-02-038 INORGANIC PREPARATIONS AMYOYIUM AZIDE / CALCIUM - GOLD ALLOY / GERMANIUM-73 SELENIDE / GERMANIUY-73 TELL 68A-09 SELENIDE / GERMANIUM-73 TELLLRIOE / NICKEL-64 - ALUMINUM ALLOY / NICKEL-61 - IRON ALLOY / POTASSIUM HEXA C 68A-OS ELLUQIOE / NICKEL-64 - ALUMINUM ALLOY / NICKEL-61 - IPON ALLOY / POTASSIUM HEXA CYAYO DI NICKELATE(I1 / PO 68A-OS ABSORPTION SPECTROPHOTOMETPY OF ALPHA EMITTING YATERIhLS/ 688-1 C-12 IA / 7IRCONIA )/ I-IGH LEVEL ALPHA RADIATION LABORATORY ( ALPHA HYDRCXY IS0 BUTYRIC ACID / BERKELIUM-249 / 688-12-01 STROLOLACTONF / 2 EETA YETFYL 19 NOR TEST0 LOLACTONE / 2 ALPHA METHYL ESTRA 4 ENE 3117 DIONE / 2 RETA YETH 688-11-04 ALPHA RADIATION DAMAGE IN INORGANIC PHOSPHORS/ 68a-oa-o~~ TRANSURPNIUM ELEMENTS / URANIA / ZIRCONIA )I HIGH LEVEL ALPHA RADIATION LABORATORY ( ALPHA HYDROXY IS0 8U 688-1 2-01 A STUDY OF PARAMETERS THAT AFFECT ANALYTICAL ALPHA SPECTRCMETRYI 68A-08-02E ASS SPFCTQUM OF CELMAN ITLC-SA MECIUM / MASS SPFCTRUM OF ALUMINA )I MASS SPECTROMETRY OF SUBSTANCES ISOLAT 6eA-07-02F ANIIJY-73 SELENIDE / CERMANIUM-73 TELLURIDE / NICKEL-64 - ALUMINUM ALLOY / NICKEL-61 - IRON ALLOY / POTASSI 684-09 AMANITA TGXINS (GALERINA MARGINATA I/ 688-02-020 NG ANC REMOVIYC OPCANIC COMPOLYDS FROM WATER ( ACETATE / AMRERLITE XAD-2 )/ EVALUATION OF A LIPOPHILIC ADS 686-02-058 TITRIYETRIC DETERMINATION OF AMERICIUM/ 68A-02-D7R F THE 4ETA 01 KETONFS OF THE LANTHANIDES AN0 ACTINIDES ( AMERICIUM / EUROPIUM / HFXA FLlJORO ACETYL ACCTqNE 68A-OZ-C7G 243 )I CONTROLLED POTENTIAL COULOMETRIC OETERMIYATIOY OF AMERICIUM ( HALF LIFE OF AMERICIUM-241 / HALF LIF 6RA-02-07A ODE I/ VOLTAMMETRIC STUDIES TF PLUTONIUMI NEPTUNIUMI AN0 AMERICIUM ( ROTATING PLATINUM DISK ELECTRODE / RO baa-02-070 CTIOY CHROMATOGRAPHIC METbOD FOR THE RAPID SEPARATION OF AMERICIUM FROM OTHER TRANSURANIUM FLEMENTS/ NEW F 68R-1 C-03 AL COULCMETRIC OETFRMINATION OF AMFRICIUM ( HALF LIFF OF AMERICIUM-241 / HALF LIFE OF AMERICIUM-243 )I CON 6 ea- o 2-0 74 PURIFICPTION OF AMERICIUM-241 AND AMFRICIUM-2431 686-02-07H PURIFICPTION OF AMEQICIUW-241 AN0 AMERICIUM-243/ 68~1-0z-07~ OF AYERICIUM ( HALF LIFt OF AMERICIUM-241 / HALF LIFE OF AWERICIUY-243 )I CCNTROLLFD POTENTIAL COULOMETRIC 688-02-076, OEUTERfl Dl METHYL SULFOXIDF / HFXA METHYL PHOSPHORIC TRI AMIDE / BARIUM PARA ETHYL RENZENE SULFONATE / EST 6 RE- 11-04 AMINO ACID SEQUENCE CF MOUSE kEMDGLDBIN/ 6PA-04-C3H AMINO ACIC SUBSTITUTICNSI t 84-04-03 I / TRI METHYL SILYL PHENYL THIO HYCANTOIN DERIVATIVES OF AMINO ACIDS )I BICMEOICAL APPLICATIONS ( FREF FAT 68A-02-010 HORIC ACID / HOEHP / LIQUID ION EXCHANGERS )I RECLAIMIhG AMINO ACIDS - CARBON-14 ( 01 2 ETHYL HEXYL ORTHO 68b-04-01G NO ACIDS )/ eICMEDICAL APPLICATIONS I FREE FATTY ACIDS / AMINO ACICS / PHFNYL THI'J HYCANTOIN DERIVATIVES 0 ~~A-OZ-C~D IDS I AMINT~ acios I PHENYL THIO HYDANTOIN DERIVATIVES OF AMINO ACIDS I TRI METHYL SILYL PHENYL THIO HYOPNT 68A-02-010 / CETERMINATION OF SUBNANOMOLE QUANTITIES OF L AMINO ACIDS BY ISOTOPE DILUTION - AMINO ACYLATION 684-04-01L NOMOLE QU4NTITIES OF L 8MlNO ACIOS RY ISOTOPE DILUTICN - AMINO ACYLATION/ DETERMINATION OF SURNA 688-04-01L RNP )I KINETICS OF AMINO ACYLATION OF TRANSFER RIB0 NUCLEIC ACID I T 68A-04-016 I PHENYL PHOSPHITF NICKEL(Cl I/ INORGANIC PREPARATIONS I AHMONIUN AZIDE / CALCIUM - GOLD ALLOY / GERMANIUM 68A-09 / OFTERMINATION OF CADMIUM IN PLUTONIUM I 4PHONIUM PYRROLIDINE 01 THIO CARRAMLTE ( APOC I I 68A-05-048 AT ORNLl OPERATIOYdL AMPLIFIER SYSTEMS IN ELECTROANALYTICAL CHEMISTRY 6EPRR-lC1 A STUDY OF PARAMETERS THAT AFFECT ANALYTICAL PLPHA SPECTRCMETRYl 68A-08-02E OMATICY / CIRCUIT TESTS / D.M.E. / ENSFMBLE AVERAGING I/ ANALYTICAL APPLICATICNS OF A DIGITAL INSTRUMENT C 68A-01-21 ANALYTICAL APPLICATIONS OF CERENKOV RADIATION/ 68A-08-028 PRECISION PHOTCMETRY bSING A PAOIOISOTOPIC LIGHT SOURCE/ ANALYTICAL APPLICATIONS OF THE SFCONOARY EFFECTS 68PRR-031 NTER ACTIVIT I ESI SPECIAL ANALYTICAL ASSISTANCE FOR ISOTOPES OEVELCPMENT CE 688-08-066 ANALYTICAL 81 CCHEMISTRY/ 68A-04 RNA / FILTER PAPER DISK TECHNIQIJE l/ INSTRUMENTATION FOR ANALYTICAL BIOCHEMISTRY ( TRANSFER RIB0 NUCLFIC A 681-01-19 A COMPARISON OF METHODS OF ANALYTICAL CHEMISTRY/ 68PRR-102 ANALYTICAL CHEMISTRY/ 68PRR-122 ODULES )I COMPUTER ASSISTED ANALYTICAL CHEMISTRY ( DIGITAL COMPUTER / LOGIC M 68A-01-20 ORT F3R PFRIOD ENDING OCT.31.1967/ ANALYTICAL CHEMISTRY CIVISION ANNUAL PROGRESS REP 68PRP-055 OPTS 1964-1067/ CUMULATIVE INOEXES TO THE ANALYTICAL CHEMISTRY DIVISION ANNUAL PROGRFSS REP 68PRP-056 STATISTICAL QUALITY CONTROL REPOPT, ANALYTICAL CHEMISTRY OIVISIONI PPR.-JUNEv1968/ 68PRR-042 STATISTICAL QUALITY CONTROL REPORT, ANALYTICAL CHEMISTRY DIVISIONt JAN.-MAR.,1968/ 68PRR-C41 STATISTICAL QUALITY CONTROL REPORT. ANALYTICAL CHEMISTRY OIVISIONI JULY-SEPT.v1967/ 68PRR-039 STATISTICAL QUCLITY CCNTROL REPORT, ANALYTICAL CHEMISTRY OIVISIONi OCT.-OEC.r1967/ 68PRR-C40 ANALYTICAL CHEMISTRY FOR REACTOR PROJECTS/ 684-03 CYNOPSIS OF ELEVENTH CCNFERENCE ON ANALYTICAL CHEMISTRY IN NUCLEAR TECHNOLOGY/ 68PRR-E32 S@OK REVIEW OF, ANALYTICAL CHEMISTRY OF PLUTONIUM/ 68PRR-035 THE ANALYTICAL CHEMISTRY OF THE ACTINIDE ELEMENTS/ EBPRR-CS7 Y.1068 I JUNE11968 / JULY7196e / hUG.91968 / SEPT.r1968/ 4NALYTICAL CHEMISTRY RESEARCH AND DEVELOPMENT MON 6RPRR-060 ANALYTICAL IMSTRUMENTATION/ 68A-01 INSTRUMFNTATION FOR THE HIGH RAOIATION LEVEL ANALYTICAL LAROPATORY I HRLAL )I sen-01-03 ORNL MASTER ANALYTICAL MANUAL/ 6BC ORNL MASTER ANALYTICAL MANUAL/ 68C-13 CUMULATIVF INDEXFS TO THE OPNL MASTER ANALYTICAL MANUAL/ 68C- 13-01 MAINTENPNCE OF THE ORNL MASTER ANALYTICAL MANUAL/ 68C-13-02 ANALYTICAL METHOOOLOCY/ 681-02 EFFECTS OF RAOIATION ON ANALYTICLL METHODS/ sen-08-07 THE FFFFCT OF RADIATION ON SOME ANALYTICAL METHODS/ 68PRR-126 LTEN FLUOPIOF SALTS/ ANALYTICAL METHODS FOR THE IN-LINE ANALYSIS OF MO 686-03-02 RAOIOLYSIS OF ACID CHLORIDE SOLUTIONS AND ITS EFFECT ON ANALYTICAL PROCEDURES/ CHLORINE PRODUCTION BY GAM 68PRR-Dl9 FFFECT OF RACIATION ON COMYOY ANALYTICAL REAGENTS/ ~BA-OR-O~F ANALYTICAL RESEARCH/ 684 NG DISCRETE SAMPLES FRCM THE CUTPUT OF A CONTINUOUS FLOW ANALYZER/ AN AUTOMATIC SAMPLER FOR OBTAIN1 68PRR-021 STS OF REACTOR FUEL ELEMFNTS ( MONOPOLE 600 RESIDUAL GAS ANALYZER )I ANALYSIS OF PURGE GAS FROM IN REACTOR 68a-03-c3a

N AN0 .INSTAL1 . __ ATlON OF PERKIN - ELMER YODEL-240 ELEMENTAL ANALYZER IN A GLOVE BOX ( CARRClN / HYDROGEN / NIT 680-02-07E~~ MOLFCULAR ANATOMY PROGRAM/ 68A-04-03 THE RAPID SEPARATION CF FERKELIUM(IVl FROM CERIUM(IVl BY ANlCN EXCHANGE/ NEW METHOD FOR 688-10-01 THE RAPID SEPARATION OF BERKELIUM(IVl FROM CERIUMlIVl BY ANION EXCHANGE/ NEW METHOD FOR 68PRR-024 121

IOFNTIFICATION OF URINARY CONSTITUENTS ISOLATED BY ANION EXCHANGE CHROMATOGRAPHY/ 6PA-04-03A FRACTIONATION Oc URINE BY GEL AN0 ANION EXCHANGE CHRCMATOGRAPHYI 6PA-04-03C IDENTIFICATION OF URINPRY CONSTITUENTS ISOLATED @Y ANION EXChANGE CHRCMATOGRAPHYl 68PRR-C10 IDENTIFICATION OF UPINARY CONSTITUENTS ISOLATE0 BY ANION EXCHANGE CHROMATOGRAPHY/ 68PRR-086 / ANION EXCHINGE CHRCYATOGRAPHY OF HYDROLYZED URINE 688-04-038 GIS CHROKATOGRAPHIC ANALYSIS OF FRACTIONS FROM THE PNIGN EXCHANGE CHRCMCTOERAPHY OF URINE/ 68A-04-030 Y OF URINE COMPONENTS I/ DESALTING OF FPICTI'ONS FROM THE ANI'3N EXCHAIIGE CHRCVATOGRAPHY OF URINE ( MASS SPE 68A-04-03E 967/ ANALYTICAL CHEMISTRY r)IVISION ANNUAL PRCGRESS REPORT FOR PERIOG ENGING OCT.31,l 68PRR-C55 CUMULhTIVE INCEXES TO THE ANALYTICAL CHEMISTRY DIVISION ANNUPL PRCGRESS REPORTS 1964-1967/ 6 8 P R R - 0 5 6 -10n CATIOY EXCHANGE RESIN I/ COLUMN CHROMATOGRAPHY WITH ANTIMONY PENTA OYICE I SEPARATION OF SODIUM / CHE 686-02-05A IN PLUTONIUM ( AYMONIUM PYPPOLIOINE DI THIO CARBAMATE I APOC I I/ DETERMINATION OF CADMIUM 68A-05-C4B ELECTRODES ( C.M.E. I ( FIRST DERIVATIVE POLAROGRAPHY I/ APPARATUS FOR PKECISE CONTROL OF MERCURY FLOW RAT 686-01-C4 SOME APPWOACHES TO MORC RAPIU ANALYSIS/ 68PRR-091 ,1967 / nEC.,lS67 / JPN.llStP / FER.. 1966 / MAR.,196R I APR.tl968 / MAY11968 / JUNE.1968 / JULY.19tB / AU 68PRR-OC0 L QUALITY CONTROL REPORT, ANALYTICAL CHEMISTRY OIVISIONT APR.-JUNEv1968/ STATISTIC4 6ePRR-042 POLAROGRPPHY OF SULFU'I 01 OXIDE ( SULFITE I IN AQUEOUS HYOROFLUDRIC ACID/ 68A-02-08C AQUEOUS INJECTION GAS CHROMATOGRPPHYl 68A-C2-044, / LIQUID SCINTILLATION CCIUNTING OF WEAK ?ETA EVITTERS IN AQUEOUS SCLUTION BY USE OF TRITON X-100 IN AN O9G 68A-OE-C2G LIQUID SCINTILLATION COUNTING OF WEPK BETA EMITTERS IN AQUEOUS SOLUTIOFI USING TRITON X-loo/ 68PRR- On5 UNTING METHOD/ RUTHENIUM RPOIOACTIVITY IN AQUEOUS SCLUTISNS, PYRICINE EXTRACTION - GAMMA CO 68PR R- C 8 0 EXPLORATORY STUDIES ( GAT CHROMATOGPAPHY flF POLY NUCLEAR AROMITIC HYOFCCARRONS. PLKALOIOS, PHENOLS, AN@ AC 68k-02-03A TOTAL PLUTONIUM - OBSERVATICNS ON THE REACTIONS SETWEEN AQSFNAZO AN0 PLUTCNIUMIIIII~PLUTONIUM(IV1 AN0 PL 68PRR-038 CHEMICAL PRECONCENTRATION OF TRACE ELEMENTS IN BONE ASH/ 68A-05-03 POSSIBLE LOSS OF CESIUM DURING ASHING OF BONFf 688-05-03C OETERMINITION OF L ASPARAGINPSEl 686-04-01K OM 9TDGXAPHVI TERMINAL NUCLEOSIDE ASSAY OF RIB0 NUCLEIC ACIC RY LIGAND EXCHANGE CHR 684-04-011 CMITOGRAPHY/ TERMINAL NUCLEOSIDE ASSAY OF RIBO NUCLEIC PCIO BY LIGANO EXCHANGE CHR 68PRR-009 NUCLEIC PCIOS BY LIGAN3 EXCHANGE CHROMATOGRAPHY/ ASSAY OF 3/ TFRMlhAL NUCLEOSIDES OF TRANSFER RIBO 68PRR-OB5 / LOGIC 8YOOIILES I/ COMPUTFR ASSISTED ANALYTICAL CHEMISTRY ( DIGITAL COMPUTER 6BA-01-20 TQFNn. ..TQ ATOMIC POWER GENERATION AN0 URANIUM RESOURCES/ 68TP-02 R.11968 / APR.,1468 / YAY,lSCB / JUNE11968 / JULYIlS68 / AUG.91968 / SEPT.,1968/ ANALYTICAL CHEMISTRY RESE 68PRR-060 N TRAVEL TO CZECbOSLOVAKlA, YUGOSLPVIA, AUSTRIA, GREECE, AUG.29-CCT.Brl967/ RFPORT OF FOREIG 68PRR-043 REPORT OF FOREIGN TRAVEL TO AUSTRALIA. FEB.1-Yr3R.71196B/ 6ePRR-C44 REPORT OF FOREIGN TRAVEL TO CZECHOSLOVAKIA^ YUGOSLAVIA, AUSTRIA7 GREECE, AUG.29-OCT.B71967/ 68PRR-043 UTRCPHIC WATER SY5TEMS ( PHOSPHATE / NITRATE / TECHNICON AUTOANALYZER / HYOROPONIC BEDS / ALGAL NUTPIENTS 684-02-048 ACIOS ( TRNA I/ AUTOMATE0 DETERMINATION OF TRANSFEQ RIRC NUCLEIC 68A-04-010 AUTOYATIC POTENTIOMETRIC TITRATOR/ 68PRR-052 , ORNL MOOEL-Q-172e AND MOOEL-Q-1728Af AUTOMATIC POTENTICMETRIC TITRATOR, VELOCITY SERVO 6BPRR-07R FROM THE OUTPUT OF A CONTINUOUS FLOW ANALYZER/ AN AUTOMATIC SAMPLEP FOR OBTAINING OISCQETF SAMPLES fRPRR-021 TEM ( P3LAROGRAPHY / FLAME PI-OTOMETRY / SIGNAL AVERAGING PUTOMATION / CIRCUIT TFSTS / O.M.E. / ENSEMBLE AV 68A-01-21 S/ PVPILABILITY OF STANOAROS FOR COMMON QAOIONUCLIOE 68PRR-CZB AVFRPGING PUTOKATION / CIRCUIT TESTS / D.M.E. / ENSEMBLE AVEQAGING I/ ANALYTICAL APPLICATIONS OF A DIGITAL 68A-01-21 AROGRPPHSl DESIGN OF TIME AVERAGING IN0 TIME OFPIVATIVE CIRCUITS COR OC POL 68A-01-10 MPUTER ZYSTEM ( POLAROGRAPHY / FLAME PHOTOMETRY / SIGNAL AVERAGING AUTCHATICN / CIRCUIT TESTS / O.M.E. / E 686-01-21 PHOSPHITE NICKEL(O1 I/ INOFGPNIC PREPPRATIONS I AMMONIUM AZIDE / CALCIUM - GOLD ALLOY / GERMANIUM-73 SELEN 688-09 N PER CHLORATE MEDIA 111. RESCLUTION OF THE ULTRAVIOLET SAND STRUCTURE - SOME CONCLUSIONS CONCERNING THE 68PRR-OOR 01 METHYL SULFOXIDE I tExn METHYL PHOSPHOPIC TRI AMIOE I BARIUM PARA ETHYL BENZENE SULFONATE / ESTROLOLACT 6 88- 11-04 GPMMA-RAY INTENSITIES IN THE OECPY OF 9ARIUM-133/ 68A-08-03F IZATION OF ISOTOPE MATERIALS ( OEC4Y SCHEMES / IRON-59 / BARIUY-140 / SAMARIUY-151 / RPOOIUM-103M / RUBIOI 6BA-08-060 E - CELLULOSE / NUCLEOSIDES / NUCLEOTIOFS / NUCLEIC ACIO BPSEZ I/ CONSTITUENTS OF TRANSFER RIBO NUCLEIC AC 68A-02-0ZC ELLULOSE/ RESOLUTION OF CCMPLEX MIXTURES OF NUCLEIC ACIO RPSES? NUCLEOSIDESI AN0 NUCLEOTIDES BY TliC OIMENS 68PRR-027 BASIC CONCEPTS OF ACTIVATION ANALYSIS/ 68PRR-107 SOURCES CF CCNTIMINATION DURING ELECTRON BEAM MELTING/ 6BPRR-057 SOURCES OF CCNTAVINPTION DURING ELECTRON BE 4M MELT I NGI 68PRR-088 IC FMULSIONSI BEAM SPLITTER =OR USE IN CALIBRATING SPECTROGRAPH 684-05-02 IC EMULSIONS/ BEAM SPLITTER FOR USE IN CALIBRATING SPECTROGRAPH 68PRR-089 HOSPHATE / NITRATE / TECPNICON PUTOPNALYZER / HYOROPGNIC BEDS / ALGAL NUTRIENTS I/ EUTROPHIC WATER SYSTEMS 6BP-02-048 E / HEXA METhYL PHOSPHORIC TRI AMIDE / BARIUM PARA ETHYL BENZENE SULFONATC / ESTROLOLACTONE / 2 BETA METHY bee-11-04 RESONANCE SPECTROMETRY ( CIYNAYYLIOENINOENE / 01 PHENYL BENZO FULVENE / POLY METHYLENE POLY PHENYL ISO CY 688-11-C4 RAOIPTION LABORATORY ( PLPHA HYOPOXY IS0 BUTYRIC ACIO / BERKELIUM-249 / CHROMATOGRAPHY / OISSOLUTION / FU 68P-12-01 OUNTINGI CHROMATOGRAPHIC SOLVENT EXTRPCTION ISOLATICN OF BERKFLIUM-249 FROM FIGHLY RADIOACTIVE SOLUTIONS A 688-1C-02 DUNTINGl CHROMbTOGRAPHIC SOLVENT EXTPlCTION ISOLbTION OF BERKELIUM-249 FROM HIGHLY RbDIOICTIVE SOLUTIONS A 68PRR-013 NEW METHOD FOR THE RAPID SEPARATION Of EERKELIUK(1VI FROM CERIUMIIVI BY ANION EXCHANGE/ 688-1C-01 NEW METhOD FOR THE RAP10 SEPARATION OF BERKELIUMIIVI FROM CERIUMIIVI BY ANION EXCHPNGEI 68PRR-024 TRUM OF MOLYROENUM(II1 1 FLUORIDE IN LITHIUM TETRA FLUORC BERYLLITEl SPEC 68A-03-OZH RANIUM(V1 AN0 URANIUMIVII IN MOLTEN LITHIUM TETRA FLUOR0 BERYLLATE ( OISPROPORTIONATION OF URANIUM(IV1 IN 6RA-03-02E INATION I OETERMINATION OF OXIDE IN LITHIUM TETRA FLUOPC BERYLLATE AN0 IN LITHIUM FLUORIDE - URANIUMIIVI-2 6 @A-0 3-01 A S OF HFLIUM-3 PARTICLES WITI' BORONt NITROGEN, SCOIUP AN0 BERY LL IUMf INTERACTION 68PRR-015 PORTIONATIOY OF URANIUM(IV1 IN MOLTEN LITHIUM FLUORIDE - BERYLLIUM FLUORIDE I/ SPECTRbL STUDIES OF URANIUM 68A-03-02E OF TEYPERATURES ON THE SPECTRUM Of URANIUMl4+1 IN MOLTEN BERYLLIUM FLUOPIOE - LITHIUM FLUORIDE MIXTU7ESI C 6RPRP.-006 AL RECUCTION OF URANILMIIV) IN MOLTEN LITHIUM FLUORIDE - BERYLLIUM FLUORIDE - ZIRCONIUM FLUORIDE ( 65.6-29 68PRR-022 TROREOUCTION OF URANIUMIIVI IN MOLTEN LITHIUM FLUORIDE - BERYLLIUM FLUORIDE - ZIRCONIUM FLUORICE AT FAST S 68PRR-108 ICALLY GENERATED URANIUM(V1 IN MOLTEN LITHIUM FLUORIDE - BERYLLIUM FLUORIOE - ZIRCONIUM FLUORIDE AT 500C/ 68A-03-024 VOLTAMMETRY OF CHROMIUMIIII IN MOLTEN LITHIUM FLUORIDE - BEPYLLIUM FLUORIDE - ZIRCONIUM FLUORIDE AT 500CI 68A-03-028 ICALLY GENERATED URANIUMIVI IN MOLTEN LITHIUM FLUORIDE - BERYLLIUM FLUORIDE - ZIRCONIUM FLUORIDE AT 500CI 68PRR-023 DCALLY GENERATED URANIUM(V1 IN MOLTEN LITHIUM FLUORIDE - BE YLLIUM FLUORIDE - ZIQCONIUH FLUORIDE AT 500CI 68PRR-109 RIC STUOIES OF CHROMIUMIIII IN MOLTEN LITHIUM FLUORIDE - &LLIUM FLUORIDE - Zi~CONiUMFLUORIDE AT 5ooci 6BPRR-110 DETERMINATION OF TRACES OF BICMUTH IN LITHIUM FLUORIDE - BERYLLIUM FLUORIDE MIXTURES/ 6BA-05-04C SYSTEM/ APPLICATIONS OF A BERYLLIUM WINDOW GERMANIUM - LITHIUM SPECTROMETER 68A-08-03C PRCPORTI ONAL BETA COUNTER, WINDOWLESS/ 6BPRR-079 OM HIGHLY RADIOACTIVE SOLUTIONS AN0 ITS DETERMINATION BY BETA COUNTING/ CHRCMAT9GRAPHIC SOLVENT EXTRACTION 688-10-02 OM HIGHLY RACIOACTIVE SOLUTIONS AND ITS OETERMINITION BY BETA COUNTING/ CHPOMATOGRAPHIC SOLVENT EXTRACTION 6BPRR-013 LOW LEVEL BETA OETECTORl 68A-08-02F HYL 3-5 HEPTANE OIONE I/ PREPARATION AND ANALYSIS OF THF BETA 01 KETONES OF THE LANTHANIDES AN0 ACTINIDES 68A-02-076 AN ORGANIC SYSTEM/ LIQUID SCINTILLATION COUNTING OF WEAK BFTA EMITTERS IN 4QUEOUS SOLUTION BY USE OF TRITO 68A-08-O2G 1001 LIQUID SCINTILLPTION COUNTING OF hEAK BETA EMITTEQS IN AQUEOUS SOLUTION USIYG TRITOY X- 68PRR-045 TC LOLACTONE / 2 ALPHA METHYL ESTRA 4 ENE 3.17 OIONE I 2 BETA METHYL ESTRA 4 €NE 3.17 OIONE / 01 BROMO FLU 688-1 1-04 BARIUM PARA ETHYL BENZENE SULFONATE I ESTROLOLACTONE / 2 BET4 METHYL 19 NOR TEST0 LOLbCTONE / 2 ALPHA METH 688-1 1-04 BIOCHEMICAL ANPLYSESl 688-1 0-08 Y FLUIDS ANALYSES PROGRAM I/ POLAROGRAPHIC SURVEY OF BIOCHECICALS ( OIFFERENTIAL GC POLAROGRAPHY / BOO 684-01-08 4NAL Y T I C 4 L R I OCHE M I ST RY / 68A-04 R PAPER CISK TECkNIQLIE I/ INSTRUMENTATIO% FOR ANALYTICAL BIOCHEPISTRY I TRANSFER RIBO NUCLEIC ACIDS / TRAN 688-01-19 APHYl SEPARATION OF COMPOUNOS OF BIOLOGICAL INTEREST BY LIGANO EXCHANGE CHROHATOGR 68A-04-028 ILYL PHENYL ThIO HYCANTCIN DERIVATIVES OF AMINO ACIDS )/ EICMEDICAL APPLICATIONS ( FREE FATTY ACIDS / AMIN 684-02-010 INSTRUMENT FOR END POINT DETECTION IN BIPOTENTICMLTRIC TITRATIOhS/ 68A-01-11 THIN FILM MERCURY ELECTRODE VDLTAMMETRY OF BISMUTH/ 68@-1C-10 ORIUM / URANIUM NITRICE )I GENERAL ANALYSES LABORATORY ( 9ISMUTH / BULK D'NSITY / CYAYIDE / FLUORIDE I POT 688-12-02 DETERMINATION OF TRACES OF RARE EARTH ELEMENTS IN BISMUTH ( CARRIER FREE PROCEGURF I/ 684- 0 5-04A MIXTURES/ OETERMINATION OF TRACES CF BISMUTH IN LITHIUM FLUORIDE - BERYLLIUM FLUORIDE 688-0 5-04C BLANKS/ 68A-05-05D SCENCE OF STEROIDS I/ STEROIDS ( GELHAN ITLC-SA MEDIUY / BOOY FLUICS ANBLYSES / FLUORESCENCE OF STFPOIDS / 684-02-02F SURVEY OF BIOCHEMICALS ( DIFFERENTIAL DC POLAROGRAPHY / BODY FLIJIDS ANALYSFS PROGRAM )I POLAROGRAPHIC 6BA-01-06 CALCULATION OF SENSITIVITIES, INTERFERENCFS, AND OPTIMUM BCMBARDINC EhERCIFS IN HELIUM-3 PCTIVATION ANPLYS 68PRR-03C POSSIBLE LOSS OF CESIUM DURING ASHING CF BONE/ 68A-05-03C CHEMICAL PRECONCENTRATION OF TRACE ELEMENTS Ih BONE ASH/ 686-05-03 / BOOK REVIEW OF, ANALYTICPL CHEMISTRY OF PLUT'INIUM 68PRR-035 GRAVIMETRIC DETERMINATION OF TETRA FLUORC BORATE WITH NITRDNl 688-10-05 INTERACTICNS OF HELIUM-3 PARTICLES WITH BORON, NITROGEN, SCDIUY AND BERYLLIUM/ 68PRR-CIS F PERKIN - ELMER MOCEL-240 ELEMENTAL ANALYZER IN A GLOVE BOX ( CARBON / HYCROGEN / NITROGEN )I MOOIFICATIO 6PA-02-07E NEUTRON PCTIVATION ANPLYSIS OF BRAIN TISSUE Foil COPPER AND MANGANESE/ 6BA-OR-OIF

E- 3.17 OIONE..~~ / 2 BETA METhYL ESTRA 4 FNE 3.17 OIONE / DI BROMO FLUGRENE / TRUYENE / UREA I VARCUM / PAPI / 6P.R-Il-C4 ANIUM NIT9IDE )I GFNERLL ANALYSES LAB'IRATORY ( BISMUTH I BULK DENSITY I CYANIDE I FLIJORI~F I PCTPSSIUY CHL ha?-12-02

METHYL~~ PFOSPHATE / 01 METHYL BUTYL PHOSPHATE / METHYL 01 BUTYL PHOSPHATE )I CETEQMIY4TION OF THE METHYL ES 66A-02-01E UTYL PHOSPHDQIC ACIDS ( TRI METHYL PHOSPHATE / DI METHYL BUTYL PHOSPHATE I METHYL OI BUTYL PHOSPHATF I/ DE 6PA-02-01E SUTYL PHOSPHATE )I DETERMINATION OF THE METHYL ESTERS OF BUTYL PHCSPHCRIC 4CIOS ( TRI METHYL PHOSPHATE / D 68A-02-01E IGH LcVEVL ALPHbL!CIATION LARORATORY I ALPHA HYDROXY IS0 BUTYRIC PCID / BERKELIUM-249 / CHROMATOGRAPHY / D 68B-12-Cl IP CARBAMATE I ADDC 1 I/ DETERMINATIO~~OF CADMIlJM IN PLlJTOhIUM ( AMMONIUM PYRROLIDINE 01 TH 6P4-05-048 .. . ~ CPLCIUM GOLD ALLOY I GERMANIUM-73 SELENIDE / GE 684-09 E NICKEL101 )/ INORGANIC PREPARATIONS ( AMMONIUM AZIDE / 1 ~~ - ~ MBARCING FNFRGIES IN HELIUM-? ACTIVATION ANALYSIS/ RAPID CALCULATION OF SENSITIVITIES, INTERFERENCEST AND 6 BP R R-G3 0 REAM SPLITTER FOR USE IN CALIBRATING SPECTROGRPPHIC EMULSIONS/ 644-05-02 BEPM SPLITTER FOR USE IN CPLIBRATING SPECTROGRAPHIC EMULSIONS/ 6@PRR-C89 SEPARATION OF CALIFORNIUM ( EINSTEINIUM )I 68A-02-07F ACTIVATION ANALYSIS WITH CALIFOPNIUM-252 NEUTRONS/ 68PRR-112 NEUTRON ACTIYATION ANPLYSIS hITH A CALIFORNIUM-252 SOURCE/ 6 EA-08-0 1C NEUTkON ACTIVATION ANALYSIS WITH C4LIFORNIUM-252 S@URCES/ 6ePRR-113 CAPABILITIES/ 68A-01-21A N OF CADMJUM IN PLUTCNIUM I AMMONIUM PYRROLIOINE DI THIO CARSAPATE I 4PDC 1 )/ DETERMINATIO 684-05-048 IN - ELMER MODEL-240 ELEMENTPL ANALYZER IN A GLCVE BOX ( CARBON / HVDP.OGEN / NITROGEN I/ MOOIFICATION 4ND 6PA-02-07E ER / INTERFERENCES TO WINKLER HFTHOO / DEAERATED WATER / CARBON DI OXIDE )/ DEAERATION SYSTEMS ( DISSOLVED 68A-OZ-C4C CPRBON-14/ 68PRR-001 71 I TQITIUM I/ QUALITY CCNTROL I RADIOPHARMACEUTICALS I CARBON--14 / THULIUM-168 / THULIUM-170 I THULIUM-! 68A-Oe-06R DEHP / LIQUID ION EXCHANGERS )I RECLAIMING AMINO ACIDS - CAPEON-14 I DI 2 ETHYL HEXYL ORTHO PHOSPH@RIC ACl 684-04-01G ERMINATION OF TP.LCES OF RARE EARTH ELEMENTS IN BISMUTH I CARRIER FQEE PRGCECURE 1/ GET 6@4-05-C4A XENE / UREA / VARCUM / PAPI / FURFURAL / HIPPURIC ACID / CARYOPHYLLENE / LIPIDS I/ NUCLEAR MAGNETIC RESONA 68R-11-04 URINARY CONSTITUENTS AND RELATED COMPOUNDS/ CATALOG OF GAS CHROMATOGRAPHIC RETENTION DATA FCR 6RPRR-037 ANTIMONY PFNTA OXIDE ( SEPARATION OF SODIUM / CHELEX-100 CATION EXCHANGE RESIN I/ COLUMN CHRWATDGRAPHY WI 68A-02-05A POTENTIAL POLAROGRAPHY/ A CELL DESIGN FOR MINIMIZING IR ERROR IN CONTROLLED 68PRR-083 CONTAINERS' FOR MOLTEN FLUORIDE SALTS I DIAMOND WINDOWED CELL FCR SPECTROPHOTCMETRIC MEASUREMENTS OF MOLTE 68A-03-CZF NSIDNAL THIN LAYER CkRDMATOGRAPHY ON POLY ETHYLENE IMINE CELLULOSE/ RESOLUTION OF COMPLEX MIXTURES OF NUCL 68PRR-027 FLUOR0 ETHYLENE / MASS SPECTRUM OF POLY ETHYLENE IMINE - CELLULCSE / MASS SPECTRUM OF SEPHADEX-G-75 / MASS 68A-D2-C2F NSFER RIB0 NUCLEIC ACID ( TRNA ) ( POLY ETHYLENE IMINE - CELLULOSE / NUCLEOSIDES I NUCLEOTIDES / NUCLEIC A 68A-02-02C SPECIAL ANALYTICAL ASSISTANCE FOR ISOTOPES DEVELOPMENT CENTER ACTIVITIES/ tRA-DP-06G CENTRIPHORESIS/ 68A-04-03G ANALYTICAL APPLICATIONS OF CERENKCV RADIATION/ 6aA-08-DZA EW METHOD FOR THE RAPID SEPARATICN OF BERKELIUYIIV) FROM CERIUM(1V) 8Y ANION EXCHANGE/ N 686-1C-01 EW METHOD FOP, THE RAPID SEPARATION OF BERKELIUMIIVJ FROM CERIUM(1V) RY ANION EXCHANGE/ N bRDRR-C24 POSSIRLE LCSS OF CESIUM DUPING PSHING OF RON€/ 684-05-03C TERBIUI4-1721 INVESTIGATION OF GPMMA-RAYS IN THE DECAY CHAIN HAFNIUM-172 GOES TO -172 GOES TO YT 6PPRR-115 SISl IYFLUENCE OF CHANNELING IN CUSTOMARY HELIUM-3 ACTIVATION AYALY 6 PA- 0 8-0 1D / IODINE-129 / IODINE-130 / -91 / THULIUM-170 )/ CHARACTERIZATION OF ISOTOPE MATERIALS I DECAY SCH 68A-08-06D NSPTESl CHARACTERIZATION OF TOBACCO SMOKE AND SMOKE CONDE 68A-02-C3 NSITES/ CHARACTERIZATION OF TOeACCO SMOKE AND SMOKE CONOE bee-1 c-i 1 IPLES OF LIGANC EXCHINCE C+ROMATOGRAPHY ON COPPER LOADED CHELEX RESIN COLUMNS/ PP INC 686-04-026 RAPHY WITH ANTIMONY PENTA OXIDE ( SEPARATION OF SODIUM / CHELEX-100 CATION EXCHANGE RESIN )I COLUMN CHROMA 68A-02-05A I TPNA )I CHEMICAL ANALYSIS CF TRANSFER RIB0 NUCLEIC ACIDS 68A-04-01H WHAT INDUSTRY EXPECTS OF THE GRADUATE IN CHEMISTRY OR CHEMICAL ENGINEERING/ 68PRR-090 YISCELLANEOUS TRACE DETERMINATIONS INVOLVING CHEMICAL PREiONCEYTRATIONl 68A-D5-C4 NE ASH/ CHEMICAL PRECONCENTRATION OF TRACE ELEMENTS IN BO 686-05-03 A CCMPbPISON OF METHODS OF ANALYTICAL CHEMISTRY/ 68PRR-102 ANALYTICAL CHEMISTRY/ h8PRR-122 COMPUTER ASSISTED ANALYTICAL CHEMISTRY I DIGITAL COMPUTER / LOGIC MODULES )I 6BA-Dl-2C OPERATIONAL AMPLIFIER SYSTEMS IN ELECTROANALYTICPL CHEMISTRY AT ORNL/ 68PRR-101 IO0 ENDING DCT.31r19tl/ ANALYTICAL CHEMISTRY DIVISION ANNUAL PROGRESS REPORT FOR PER bBPRR-C55 967/ CUMULATIVE INDEXES TO THE ANALYTICAL CHEMISTRY DIVISION ANNUAL PRDGRESS REP'IRTS 1964-1 68PRP-056 STATISTICAL QUALITY CONTROL REPORT, ANALYTICAL CHEMISTRY DIVISION, APR.-JUNE.l96P/ 68PRR-C42 STATISTICAL QUALITY CONTROL REPORT, ANALYTICAL CHEMISTRY CIVISIONI JAN--MAR.r1968/ 68PRR-041 STATISTICAL PUALITY CONTROL RFPORTI ANALYTICAL CHEMISTRY DIVI.SlONt JULY-SFPT.v1967/ 68PRR-C39 STATISTICAL QUALITY CONTROL REPOPTI ANALYTICAL CHEMISTRY DIVISION, OCT.-DEC.,1967/ 68PRR-040 ANALYTICAL CHEMISTRY FOR REACTGR PROJECTS/ CBA-03 SYNOPSIS OF ELEVENTH CONFERENCF ON ANALYTICAL CHEMISTRY IN NUCLEAR TECHNOLOGY/ 68PRR-C32 BOOK REVIEW OF, ANALYTICAL CHEMISTRY OF PLUTONIUM/ 68PRR-035 THE ANALYTICAL CHEMISTRY OF THE ACTINIDE ELEMENTS/ 6ePRR-097 WHAT INDUSTRY EXPECTS OF THE GPAOUATE IN CHEMISTRY OR CHFMICAL ENGINEERING/ 68PRR-CSO NE.1968 / JULYI1S68 / AUG.rl9tB / SEPT.r1968/ ANALYTICAL CHEMISTRY RESEARCH AN0 CEVELOPMENT MONTHLY SUMMAA 68PRR-060 STATE OF URANYL ION/ ABSORPTION OF THE URANYL ION IN PER CHLORATE MEDIA 111. RESOLUTION OF THE ULTRAVIDLE 6BPRR-C08 RADIOLYSIS OF PER CHLORIC ACID/ 6eA-Oe-07C BISMUTH / BULK DENSITY / CYANIDE / FLUORIDE I POTASSIUM CHLORIDE / OXYGEN / PYCNOMETEP / SFALED TURF DISS 686-1 2-02 CEDVRESl CHLORINE PROOUCTION BY GAMMA RIDIOLYSIS OF ACID CHLORIDE SOLUTIONS AND ITS EFFECT ON ANALYTICAL P 68PRR-019 CONCENTRATING HYDROCHLORIC ACID I HYDROGEN CHLORIDE-36 / CONTROLLFD CIEHYDRATION )I 684-92-050 DRIDE SOLUTIONS AND ITS EFFECT ON ANALYTICAL PROCEDURES/ CHLORINE PRODUCTION BY GAMMA RJCIOLYSIS Oc ACID C OBPRR-C1S VE GAS CHROMATOGRAPHY I VARIAN-AERDGRAPH PREPARATIVE GAS CHROMATOGRAPH )I PREPARATI 686-02-016 ION EXCHANGE Ct-ROHATOGRAPHY OF URINE/ GAS CHROMATOGRAPHIC ANALYSIS OF FRACTIONS FROM THE AN 68A-04-03D DERIVATIVE GAS CHROMATOGRAPHY ( GAS CHROMATOGRAPHIC OETECTOR SPECIFIC FOR SILICCN )I 68A-02-01H ERICIUM FROM OTHER TRANSURANIUM ELEMENTS/ NEW EXTRACTION CHRCMATOGRAPHlC METHOD FOR THE RAPID SEPARhTION 0 689-1C-03 TUENTS AND RELATED COMPOUNDS/ CATALOG OF GAS CHROMATOGRAPHIC RET€NTION DATA FOR URINARY CONSTI 6ePRR-037 ACTIVF SOLUTIONS AND ITS DETERMINATION BY BETA COUNTING/ CHROMATOGRAPHIC SOLVENT EXTRACTION ISOLATION OF B 688-1 C-02 123

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ACTIVE SOLUTIONS AN0 ITS DETERYINATION RY BETA CrJUNTINGl CHROMATOGRPPHIC SOLVENT EXTRlrCTlON ISOLATION OF B 6RPRR-013 GAS CHROMATOGPAPHYI 684-02-01 A REPOOELED LABGFATORY FOR GAS CHRCMATOGPAPWYI 686-02-ClB THIN LAYFR CHQOHATOGRAPHY/ 684-02-02 THIN LAYC!? CHROMATOGRAPHY/ 68b-02-C3B AQUEOUS INJECTION GAS CHROMITOGRAPHY/ 68A-02-04A LIGANO EXCHANGE CYROMATOGRAPHYI 6861-04-02 ‘RACTICNATION OF UFINE BY GEL LND ANION FXCHANGE CHQOMATOGRPPHY/ 68A-04-03C FRACTIONATION OF HUMAN URINF BY GFL CHROMATOGRAP’iY/ 68PRR-084 ATION OF URINARY COVSTITUENTS ISOLATED BY ANION EXCHANGE CHROMATOGRAPHY/ IDENTI FIC 688-04-031 ATION OF URINARY CONSTITUENTS ISOLPTEO PY ANION EXCHANGE CHQOMATOGRAPHYI IOCNTIFIC 68PRR-C10 ATInN OF URILlAPY CCNSTITUENTS ISOLATED PY ANION EXCHANGE CHROMATOGRAPHY/ IOENTIFIC 68PRR-0P6 N CF COMPOUYCS CIF BIOLOGICAL INTEREST eY LIGAND EXCHANGE CHROMATOGRAPHY/ SEPARATIJ 684-04-028 NUCLEOSIDE ASSPY OF RIBO NUCLEIC ACIO BY LIGAND EXCHANGE CHROMATOGRAPHY/ TEPYINAL 6@A-04-011 NUCLEOSIDE ASSbY OF RIB9 NUCLEIC ACID FY LIGAND EXCHANGF CHRGPATOGRAPHY/ TERMINAL 68PRP-OC9 OSIOES OF TRANSFER RIB@ NUCLEIC ACIDS @Y LIGAND EXCHANGE CHRCMATOGRAPWY I ASSAY OF 3/ TERMINAL NUCLF 6BPRR-C85 ATORY I ALPHA HYDROXY IS0 EUTYRIC ACID / BiqKELIUM-24? / CHROMATOGRAPPY / DISSOLUTION / FUSION I ION EXCHA 688-12-01 CIFIC FOR SILICON )I ClERIVATIVE GAS CHROCATOSRAPHY I GAS CHROMATOGRAPHIC DETECTOR SPF 68A-02-01H / MASS SPECTROMETRY OF SUBSTCNCES ISOLATED BY THIN LAYER CHROMATOGRAPHY I MASS SPECTRUM OF POLY TETRA FLU0 68A-02-02F CHROPATOGQAPF I/ PREPARATIVE GAS CHROMATOGRAPHY ( VIRIAN-AEROGRAPH PREPARATIVE GAS 686-02-016 FRARFO SPCCTROMETRY OF SUBSTANCES ISOLATED BY THIN LAYFR CHRCMATOGRAPHY ( UICK-STICKS I/ IN 6BA-02-02G GEL PERMEATION CHROMATOGRAPHY AS A SEPARATIONS TECHNIQUE1 688-10-IIC ANION EXCHANGE CHRCMATOGRAPHY OF HYDROLYZED URINE/ 68A-04-038 KALOIOS. PHEYOLS, AN0 ACIDS I/ EXPLOR4TCRY STUOIFS I GIS CHROMATOGRAPHY OF POLY NUCLEAR AROMATIC HYOROCARB 684-02-03A ATDFRAPHIC ANALYSIS OF FRACTIONS FROM THE ANION CXCHANGE CHROMATOGRAPPY OF URIYEl GAS CHROM 68A-04-C30 PNFNTS I/ OESPLTING OF FRACTIONS FDOM ThE ANION EXCHANGE CHROMATOGRAPhY GF URINE ( YbSS SPECTDOMETRY OF UR 68A-04-C3E MNSl PPINCIPLES OF LIGAND EXCHANGE CHROMATOGRAPHY ON CCPPER LOADED CHELEX RESIN COLU 684-04-02 A SFPARATION OF SIX CCRTICGSTEPOIOS BY THIN LAYER CHRCMATOGPAPHY ON CFLMAN ITLC-SA MEDIUM/ 6PPRR-C76 CLFOSI’ICS, AVC NUCLCOTIOES BY THO PIMFNSIONAL THIN LAYER CHROMATOGRAPkY GN POLY ETHYLENE IMINE CELLULOSE/ 68PRR-027 N CF SOOIIJM I CHELEX-100 CATION EXCHANGE RESIN I1 CCLUMN CHROPATOGRAPHY WITH ANTIYONY PENTA OXIDE I SEPARA 68A-02-05A UM FLUOFID! - ZIRCONIUM CLUORIDE AT 500CI VOLTAHMCTRY OF CHROMIUM(1I) IN RCLTEN LITHIUM FLUORIDE - BERYLLI 68A-03-028 DE - ZIRCflNIUY FLIJOPIOE AT 5CCCI VOLTAMMETRIC STUOIES OF CHROMIUPIIII IN MOLTFN LITHIUM FLUClRICE - BEPYLLI 68PRR-110 E SOLUTION I &8SORoTION SPECTRA OF IPON(I11~NICKELIII), CHQOMIUMIIIIr AN0 CHRClMIUM(III1 IN MOLTEN FLUORIO 68A-03-02G PTICN SPECTPA OF IRON(II1~NICKEL(II1, CHROMlUMlIIl. AN0 CHROMIUM(III1 IN MOLTEN FLUORIDE SbLTS I1 ABSORPT 68A-03-02G I YqTRUYENTATlON I CHRCPOSCAN I/ 68A-02-OZA hE / LIPIGS I/ NIJCLEAR PACNETIC RESONANCE SFECTROMETRY ( CINNAPYLIDENINCENE I 01 PHENYL EENZO FULVENE / PO 688-11-04 RAPHY / FLAYE PHOTOHFTRY / SIGVAL AVFRAGING AUTOMATION / CIRCUIT TESTS / O.M.E. I ENSEMBLE AVERAGING I/ AN 68A-01-21 OFSIGN OF TIYE AVEQAGING ANC TIYE DERIVATIVE CIRCUITS FOR OC POLAPCGRAPHS/ 68A-01-10 NTROLLEO CURPENT CYCLIC VOLTAMMETER/ DERIVATIVE CIRCUITS FOR USE UlTH THE CONTROLLED POTENTIAL GO 68A-01-13 BORATOPY COMPARISON OF YEASUREMENTS OF THE RADIONUCLIDES CORALT-579 POLYBnENbM-99 - TECHNFTIUY-9qMI AN0 TE 6PA-08-03A PARATION ’IF SODIUM / CHELEX-1CO CATION EXCHANGE QESIN I/ COLUMN CHRCNATOGRAPPY WITH ANTIMONY PENTA OXIDE ( 6BA-02-056 NO EXCHANGE CHROMATOCRAPHY CN COPPER LOAOEO CHELEX RESIN COLUMNS1 PRINCIPLES OF LIGA 68A-04-026 AOVI SORY C GMH I T T E E ME C B E RS AN 0 CON S ULT AN 1S / 680- 14-01 EFFECT OF RAOIATION ON COMMON ANALYTICAL REAGECTS/ 6RA-0 8-07E AVPILABILITY OF STANDARDS F@R COMMON RbOIONUCLIOESl 68PRR-028 MODIFICATION OF DUAL SET POINT VOLTAGE COMPARATCR ( ORNL MOCFL-Q-2950 I/ 6BA-01-15 TOGRAPHY ON POLY ETHYLENF IMINE crcLuLosci RFSOLUTIGN OF COMPLEX MIXTUPES CF NUCLEIC ACIO BASES, NUCLEOSIO 68PRR-027 VGF CHROMATOGRAPkY OF URINE ( MASS SPECTROMETRY OF LRINE COMPONENTS I/ CESALTING OF FRACTIONS FROM THE ANI 6 8A-04-03E HIUY GAMYA SPECTROMETRY OF FISSION PRODUCTS DEPOSITED IN COMPONENTS OF THF MSRE/ YEASUREMENT BY GERMANIUM 68A-08-04C COMPUTER ASSISTED ANALYTICAL CHEMISTRY ( DIGITAL COMPUTER / L@GIC YOOULES I/ 686-01-20 COMPUTFR / LflGIC MOOULES I/ COMPUTER ASSISTED ANALYTICAL CHEMISTRY I DIGITAL 68A-01-20 IN THE ANALYSIS OF TRANSFER RIBO NUCLEIC ACIDS I TRNA I/ COMPUTER PROCESSING OF LIQUID SCINTILLATION COUNT 684-04-01E AGING I/ ANALYTICAL APPLICATICNS OF A DIGITAL INSTRUMENT COMPUTER SYSTEM I POLIROGRAPHY / FLAVE PHOTOMETRY 6FI-01-21 DE-36 / CONTROLLED DEI-YORATION I/ CONCENTRATING HYORCCHLORIC ACID ( HYORPGEN CHLrRI 68A-02-050 DEVICE FOR THE UNATTENDED CONCENTRATION OF SOLUTIONS/ 68A-02-05C SEPARATION AN0 CONCENTRATION STUCIESl 68A-02-C5 BASIC CONCEPTS OF ACTIVATION ANALYSIS/ 68PRR-107 111. RESOLUTION OF THE ULTRAVIOLET BAND STRUCTURE - SGME CONCLUSIONS CONCERNIXG THE cXCITEO STATE OF URANY 68PRR-008 CFARACTEPIZITION OF TOSACCO SMOKE AN0 SMOKE CONOENS AT ES/ 68A-02-03 CbARACTERIZATICN CF TOBACCO SMOKE IN0 SMOKF CONDENSATES/ 688-10-11 E MSRE FUFL BY HYDROGEN REOUCTION f ABSORPTION - THERMAL CONDUCTIVITY MEASUREMENT OF HYDROGEN FLUORIDE IN 6 PA-03-01 8 HNOLOGYl SYNOPSIS OF ELEVENTH CONFERENCE ON ANALYTIC4L CHCYISTRY IN NUCLEAQ TEC 68PRR-C32 ATALOG OF GAS CHROMATOCRAPhIC RETENTION DATA FOR URINARY CONSTITUENTS AN0 RELATED COMPOUNDS/ C 68PRR-037 RAPHYI IOENTlFICATION OF URINARY CONSTITUENTS ISOLATED BY ANION EXCHANGE CHROMbTOG 686-04-036 RAPHYl IOENTIFICATION OF URINARY CONSTITUENTS ISOLATED BY ANION EXCHANGE CHROMATOG 68PRR-010 PAPHYl IOENTIFIC4TION OF URINARY CONSTITUFhTS ISOLATED BY AVION EXCHANGE CHROMATOG 6 13 P RR- 0 86 LOSE I AlUCLECSIDES / NUCLEOTIDES / NUCLEIC ACIO EASES 11 CONSTITUENTS OF TRANSFFR 9160 NUCLEIC ACID I TRNA 6EA-02-02C ADVISORY COMMITTEE MEMBERS AN0 CONSULTANTS/ 680-14-C1 CTROPkOTOMETPIC MEASUREYENTS OF MOLTEN FLUORIDE SALTS I/ CONTAINERS FGR MOLTEN FLUORIDE SALTS I DIAMOND WI 68A-03-02F N MOLTEN PERYLLIUM FLUORIDE - LITHIUM FLUORIDE MIXTURFSl CONTAINMENT OF MOLTEN FLUORIDES IN SILICA I. EFF 68PRR-006 RAOIOACTIVE CONTAUINANTS/ 68A-05-05E SOURCES OF CONTAUINATION DURING ELECTRClN BEAM MELTING/ 68PRR-C57 SOURCES OF CONTAYINATION DURING ELECTRON BEAM WELTING/ 68PRR~088 QUALITY CONTROL/ 666-12-06 IUM-168 / THULIUM-170 / THULIUM-171 / TRITIUM I/ QUALITY CONTPOL I RAOIL!PHARMACEUTICALS / CAREON-14 I THUL ~BA-o e-066 RAOI ITION CONTROL AN0 SAFETY1 688-1 2-05 ( FIRST DERIVATIVE POLARCGRLPHY I/ APPARATUS FOR PRECISE CONTROL OF MERCURY FLOW RATE OF DROPPING MERCURY 6@A-0 1-04 R.-JUNEv 1968/ STATISTICAL QUALITY CONTROL REPORT, ANALYTICAL CHEMISTRY OIVISIONI AP 68PRR-042 N.-HAR. 7 1968/ STATISTICLL QUALITY CONTROL REPORT, ANALYTICAL CHEMISTRY OIVISIONI JA 68PRR-C41 LY-SE PT. 9 1967/ STATISTICAL QUALITY CONTROL REPORT, ANALYTICAL CHEMISTRY DIVISION9 JU OBPRR-C39 T.-0EC.r 1967/ STATISrICAL QUALITY CCNTROL REPORT, ANALYTICAL CHEMISTRY DIVISION, OC 68PRR-040 CYCLIC VOLTAMMETER. CONTROLLEC POTENTIAL, CONTROLLEC CURRENT/ 68PRR-072 CONTROLLED POTENTIAL CONTROLLED CURRENT CYCLIC VOLTAMMETFRl 68A-01-12 CONTROLLED POTENTIAL AN0 CONTROLLED CURRENT CYCLIC VOLTAMMETER/ 68PRR-051 ERIVATIVE CIRCUITS FOR USE WITH THE CONTQOLLEO POTENTIAL CONTROLLEO CURRENT CYCLIC VOLTAMMETER1 0 68A-01713 CONCENTRATING HYDROCHLORIC ACID ( HYOQOGEN CHLORIDE-36 / CONTROLLED OEHYOQATION I/ 68A-02-050 SERVO CONTROLLED PIPETTERS/ 68PRR-C54 C VOLTAMMETER1 CONTROLLED POTEYT ILL AN0 CONTROLLED CURRENT CYCLI 68PRR-051 - ADVANTAGES OF RAPID AN0 DERIVATIVE OC POLAROGRAPHY/ A CONTROLLED POTENTIAL AN0 DERIVATIVE OC POLAROGRAP 6EA-01-06 LTAMMETERl CONTROLLED POTENTIbL CONTROLLED CIJRRENT CYCLIC VO 68A-01-12 LTAYYETERI DERIVATIVE CIRCUITS FOR USE UITH THE CCNTROLLEO POTENTIPL CGNTROLLEO CURRENT CYCLIC VO 68A-01-13 LF LIFE OF AMERICIUM-241 / HALF LIFE OF A;4ERICIUM-241 I/ CONTROLLED POTENTIAL COULOMETRIC DETERMINATION OF 68A-02-07A SOLID STATE CONTROLLFO POTENTI dL COULOMETRIC TITRATOR/ 68A-0 1-01 1 24

MODEL-9-2564 )I MODIFICATIONS TO THE HIGH SFNSITIVITY CONTROLLED POTENTIAL CYJLOMETRIC TITRATOR I ORNL 68b-01-C2 42 POLAROGRAPHIC DROP TIYE CCNTROLLERl CRNL M03tL-Q-2792 CONTROLLED POTFNTIAL DC POLAROGRAPY AN0 ORNL MODE 68A-01-09 MODEL-9-27921 CONTROLLEC POTENTI DL OC POLAROGQApH VOLTAMMETER / 68PRR-050 V. SUBTRACTIVE POLAROGRAPHY/ CONTROLLED POTENTIAL DIFFERENTIAL OC POLAROGRAPHY 68PRR-C33 A CELL DESIGN FOR MINIMIZING IR ERROR IN CONTROLLED POTENTIAL POLPR!JGRAPHY/ 66PRR-Ce3 CYCLIC VOLTAMMETER, CONTROLLED POTENTIAL, CCNTROLLEO CURRENT/ 68PRR-072 L-Q-2564/ COULOMETRIC TITRATOR, CONTRGLLEO POTENTIAL. HIGH SENSITIVITY, ORNL MODE 6RPRR-077 OLAROC-RAPH ANC ORNL MODEL-Q-2942 POLAROGRAPHIC DROP TIYE CONTROLLER/ ORNL MODEL-'2-2792 CONTROLLED POTENTIA 684-01-09 POLAROGRAPHIC DROP TIME CONTROLLER / MqDEL-Q-2942/ 68PRR-049 PHOTOVOLTAIC CONVERSICN OF RAOICISOTOPE DECAY ENERGY/ 68A-08-CZB RADIONUCLIDES IN HIGH FLUX ISOTOPE REACTOR COOLANT WATER/ 686-08-0bH COOPERATIVE ISOTOPES PROGQPM I XPDIOISOTOPES )I 6RA-08-06 COOPERPTIVE PROJECTS/ 688-01-23 NEUTRON ACTIVATION AhALYSIS OF BRAIN TISSUE FOR COPPER bN0 M4NGANESEI 68A-08-01F PRINCIPLES OF LIGAND EXCHANGE CHROYCTOGRAPHY ON COPPER LOADED CHELFX RCSIN COLUMNS/ 68A-04-02A HEMICAL GENERATION AN0 SPECTROPHOTOMETRIC MEASUREYENT OF COPPER1111 IN ,MOLTEN LITHIUM FLUORIDE - SODIUM FL 68A-03-CZI / MASS SPECTRUM OF MERCK SILICA GEL G / MASS SPECTRUM OF CORNING POROUS GLASS 7935 / MASS SPECTRUM OF GELM 684-02-02F ELMAN ITLC-SA MEDIUM/ SEPARATION CF SIX CORTICCSTEROIDS 3Y THIN LAYER CHROMATOGRAPHY ON G 68PRR-C76 241 / HALF LIFE OF AMERICIUM-243 )I CONTROLLED POTENTIAL COULOMETRIC DETERMINATION OF AMERICIUM I HALF LIF 68A-02-07A SOLID STATE CONTROLLED POTENTIbL COULOMETRIC TITRPTOR/ 68A-01-01 MODIFICATION OF THE ORNL MODEL-9-2564 HIGH SENSITIVITY COULOMETRIC TITRbTORl 68PRR-048 HIGH SENSITIVITY COULOMETRIC TITRATOR / MOOEL-Q-2564/ 68PRR-053 DIFICATIONS TO THE HIGH SENSITIVITY CONTROLLED POTENTIAL COULOMETRIC TITRATOR I ORNL MODEL-'2-2564 I/ HO 684-01-02 SENSITIVITY, ORNL MODEL-Q-2564/ COULOMETRIC TITRATORI CONTROLLED POTENTIAL, HIGH 68PRR-077 PROPORTIONAL BETA COUNTERt WINDOWLESS/ 68PRR-079 THEORY AND PRACTICE OF LIQUID SCINTILLATION COUNTING/ 68PRR-117 GHLY RADIOACTIVE SOLUTIONS AND ITS DETERMINATION BY BETA COUNTING/ CHROMATOGRAPHIC SOLVENT EXTRACTION ISOL 688-10-02 GHLY RADIOACTIVE SOLUTIONS AND ITS DETERMINATION BY BETA COUNTING/ CHROMATOGRAPHIC SOLVENT EXTRACTION ISOL 68PRR-013 DS ( TRNA 11 CCMPUTER PROCESSING OF LiauIo SCINTILLATICN COUNTING DATA IN THE ANALYSIS OF TRANSFER RIBO NU 68A-04-01E NAR SAMPLES/ LOW LEVEL RADIATION COUNTING FACILITY FOR GEOCHEMICAL AND RETURNED LU 68A-08-02H TIVITY IN AQUEOUS SOLUTIONS7 PYRIDINE EXTRACTION - GAMMA COUNTING METHOD/ RUTHENIUM R A01 CAC 68PRR-080 TRITON X-100 IN AN ORGANIC SYSTEM/ LIQUID SCINTILLATION COUNTING OF WEAK BETA EMITTERS IN AQUEOUS SOLUTIO 68A-08-02G N USING TRITON X-1001 LIRUID SCINTILLATION COUNTING OF WEAK BETA EMITTERS IN AQUEOUS SOLUTIO 68PRR-045 OF INTELLECTUAL ABILITY FOR PREDICTING GRADES IN RELATEO CRAFT TRAINING/ VALIDITY OF SOME TESTS 68PRR-005 NEW NUCLEAR DATA I GAMMA-RAY ENERGIES / THERMAL NEUTRON CROSS SECTIONS I/ 68A-08-038 VISION ANNUAL PROGRESS RrPORTS 1964-1967/ CUMULPTIVE INDEXES TO THE ANALYTICAL CHEMISTRY DI 68PRR-C56 MANUAL/ CUMULATIVE INDEXES TO THE ORNL MASTER ANALYTICAL 68C-13-01 DETERMINATION OF SIL!CDN IN CURIUM OXIGE DI CURIUM-244 TRI OXIDE )I 68A- 0 5-0 5 OETERMINATICW OF SILICON IN CUQIUM OXIDE I 01 CURIUM-244 TR1 OXIDE )I 6 88-0 5- 05 CYCLIC VOLTAMMETER, CONTRCLLEO POTENTIAL, CCNTROLLEO CURRENT/ 68PRR-C72 CONTROLLED POTENTIAL CONTROLLFD CURRENT CYCLIC VOLTAMMETER/ 68A-01-12 COWTROLLED POTENTIAL AN0 CONTROLLED CURRENT CYCLIC VOLTAMMETER/ 65PRR-051 IRCUITS FOR USE WITH THE CONTROLLED POTENTIAL CONTROLLED CURRENT CYCLIC VOLTAMMETER/ DERIVATIVE C 68A-01-13 INFLUENCE OF CHANNELING IN CUSTOMARY HELIUM-3 ACTIVATION ANALYSIS/ 68A-08-01D DI PHENYL BENZO FULVENE / POLY METHYLENE POLY PHENYL IS0 CYANATE / FURFURYL ALCOHOL I FURAN ALCEHYDF / CRG 68R-11-04 M IN MIXTURES OF FLUORIDE SALTS, SPECTROPHOTOMETRIC THIO CYANATE METHOD/ NIOBIU 65PRR-C82 / GENERAL ANALYSES LABORATORY I BISMUTH / BULK DENSITY / CYANIDE / FLUORIDE / POTASSIUM CHLORIDE / OXYGEN 48B-12-02 ALUMINUM ALLOY / NICKEL-61 - IRON ALLOY / POTASSIUM HEXA CYANO 01 NICKELATEII) / POTASSIUM NICKELIIV) PPRA 684-09 M NICKELIIV) PARA PER IOCATE 1/2 WATER / POTASSIUM TETRA CYANO NICKELATEIIII / TETRA KIS TRI PHENYL PHOSPH 688-09 CONTROLLED POTENTIPL CONTROLLED CURQENT CYCLIC VCLTAMMETERl 68A-01-12 CCNTROLLED POTENTIAL AN9 CONTROLLED CURQENT CYCLIC VOLTAMMETER/ 6RPPR-051 FOR USE WITH TkE CONTROLLED POTENTIAL CONTROLLED CURRENT CYCLIC VOLTAMMETER/ DERIVATIVE CIRCUITS 68A-01-13 LEC CURRENT/ CYCLIC VOLTAMMETER, CONTROLLED POTENTIAL. CONTROL 68PRR-072 DETERMINATION OF PER FLUOR0 METHYL CYCLO HEXANE IN METHANE/ 68A-02-01F AND ENGLAND, SEPT.2-30rlSt7/ REPORT OF FORElGN TRAVEL TO CZECHOSLGVAKIAv ITALY, SWITZERLANOi GERMANY, WEST 68PRR-047 29-OCT.8r1?67/ REPORT OF FOREIGN TRAVEL TO CZECHOSLOVAKIA, YUGOSLAVIA, AUSTRIA, GREECE, PUG. 6RPRR-043 HIC STUDIES WITH THE TEFLGN OPDPPING MERCURY ELECTRCDE I D.M.E. )I POLARflGRAP 68A-02-08 OL OF MERCURY FLOW RATE CF DROPPING MERCURY ELECTRODES I D.M.E. ) I FIRST DERIVATIVE POLAROGRAPHY )I APPAR 68A-01-04 OTOMETQY / SIGNAL AVERAGING AUTOMATION / CIRCUIT TESTS / D.M.E. / ENSEMSLE 4VERAGING I/ ANALYTICAL APPLICA 68A-01-21 TA/ EVALUATION OF VERTICAL ORIFICE RAPID TEFLON D.M.E. FOR OBTPINING FUNDAYENTAL POLbROGRAPHIC DA 68A-02-08A ALPHA RADIATION DAMAGE Ih INORGANIC PHOSPHORS/ 68A-08-02C ID TEFLON D.M.E. FOR OBTAINING FUNDAMENTAL POLAROGRAPHIC DATA/ EVALUATION OF VERTICAL ORIFICE RAP 68A-02-0eA SECTIONS )I NEW NUCLEAR DATA I GAMMA-RPY ENERGIES / THERMPL NEUTRON CROSS 688-08-038 DSI CATALOG OF GAS CHROMATOGRAPHIC RETENTION DATA FOR URINARY CONSTITUENTS AND RELATED COMPOUN 68PRR-037 I/ COMPUTER PROCESSING OF LIQUID SCINTILLATION COUNTING DATA IN THE AN4LYSIS 'IF TRANSFER RIB0 NUCLEIC ACI 68A- 04- 01E MASS SPECTROMETRIC DATA REDUCTION/ 68A-06-C4 E DC POLAROGRAPHY/ A CONTROLLED POTENTIAL AND DERIVATIVE DC POLAROGRAPH - POVAYTAGES OF RAPID AND DERIVATI 68A-01-06 TIME CONTROLLER/ ORNL MODEL-Q-2792 CONTROLLED POTENTIAL DC POLAROGRAPH AND CRNL MODEL-'2-2942 POLAROGRAPHI 684-01-09 CONTROLLED POTENTIAL DC POLAROGRAPH VOLTAMMETER / MODEL-Q-2792/ 68PRR-050 ESIGN OF TIME AVERAGING AND TIME DERIVATIVE CIRCUITS FOR DC POLAROGRAPHSI 0 68A-01-10 TIVE OC POLAROGRAPH - ADVANTAGES OF QAPID AN0 DERIVATIVE DC POLAROGRAPHY/ A CONTROLLED POTENTIAL AND DERIV 6RA-01-06 CONTROLLED POTENTIAL DIFFERENTIAL DC POLAROGRAPHY V. SUBTRACTIVF POLAROGRAPHY/ 68PRR-033 POLAROGRAPHIC SURVEY OF BCOCHEMICALS ( DIFFERENTIAL OC POLAROGRAPHY / BODY FLUIDS ANALYSES PROGRAM )/ 68A-OI-CB XYGEN / SALINE WATER I INTERFERENCES TO WINKLER METHOD / DEAERATED WATER / CARRON 01 OXIDE )I DEAERATION S 68A- 02- 04C TO WINKLER METHOD I DEAERITED WATER / CARBON 01 OXIDE )I DEAERATION SYSTEMS I DISSOLVE0 OXYGEN / SALINE WA 68A-02-04C Y RESEARCH AND DEVELOPMENT MONTHLY SUMMARY - NOV.vl967 / DEC.11967 / JAN.91968 / FEB.9 1968 / MAR.71968 / 68PRR-060 TO YTTERRIUM-172/ INVESTIGATION OF GAMMA-RAYS IN THE DECAY CHAIN HAFNIUM-172 GOES TO LUTETIUM-172 GOES 68PRR-115 PHOTOVOLTAIC CONVERSION OF RADIOISOTOPE DECAY ENERGY/ 68A-08-028 GAMMA-RAY INTENSITIES IN THE DECAY OF BARIUM-133/ 68A-08-03F DECAY OF -103 - RHODIUM-l03M/ 688-08-03E / THULIUM-170 )I CHARACTERIZATION OF ISOTOPE MATERIALS I OECIY SCHEMES I IRON-59 / 9ARIUM-140 / -I 6BA-08-06D NUCLEAR SPECTROSCOPY IN THE NEUTRON DEFICIENT MASS NUMeER BETWEEN 173-185 REGION/ 68A- 08-030 NG HYCROCHLORIC ACID I HYDRGGEN CHLORIDE-36 / CCNTROLLED DEHYDRATICN I/ CONCENTRATI 68A-02-050 THE DESIGN AND EVALUATION 'IF P, DELAYED NEUTRON LEACHED HULL MONITOR/ 68PRR-059 NEW TITRANT DELIVERY UNIT bN0 ELEVATOR/ 68A-01-038 NITRIDE I/ GENERAL ANALYSES LAGORATORY I BISMUTH / BULK DENSITY / CYANIDE / FLUORIDE / POTASSIUM CHLORIDE 686-12-02 RMANIUM - LITHIUM GAMMA SPECTROMETRY OF FISSION PRODUCTS DEPOSITED IN COMPONENTS OF THE MSREl MEASUREMENT 6 8A- 0 8-04C DESIGN OF TIME AVEQAGING AND TIME DERIVATIVE CIRCUITS FOR OC POLAROGRAPHSl 68A-01-10 OTENTIAL CONTROCLEC CURRENT CYCLIC VOLTIMMETERl DEPIVATIVE CIRCUITS FOR USE WITH THE CONTROLLED P 688-01-13 D DERIVATIVE DC POLAROGRAPHY/ A CONTROLLED POrENTIbL AND DERIVATIVE DC POLAROGRAPH - ADVANTAGES OF RAPID A 68A- 01- 06 AND DERIVATIVE DC POLAROGRAPH - ADVANTAGES OF RAPID AND DERIVATIVE DC POLAROGRAPHY/ A CONTROLLED POTENTIA 6 8A-01-06 IC DETECTOR SPECIFIC FOR SILICON )I DERIVATIVE GPS CHROMATOGPAPHY ,( GAS CHROMATOGRAPH 68A-02-01H W RATE OF DROPPING MERCURY ELECTRODES I 0.M.E. 1 I FIRST DERIVATIVE POLAROGRAPHY I/ APPARATUS FOR PRECISE 68A-01-04 125

A

OF AMINO ACICS I TRI METHYL SILYL PHENYL THIO HYDANTOIN DEPIVATIVES OF AMINO ACIDS I/ BIOMEDICAL APPLICAT 60A-02-010 ( FREE FATTY ACIDS / AMINO ACIOS / PHENYL THIO HYDANTOIN DERIVATIVES @F WINO ACIDS / TRI METHYL SILYL PHE 68A-02-010 XAC-2 )I EVALUATION OF 4 LIPOPHILIC EDSOF'DTION 9ESIN FOR OESPLTING AND RFMDVING ORGANIC COMPOUNDS FPOM WAT 68A-02-058 APHY OF URINE ( MASS SPECTRCYETPY OF U':IPIE CDYPDNCNTS I/ DESALTING OF FRACTIONS FROM THE ANION EXCHANGE CH 60A-04-03E D PULL MONITOR/ THE OFSIGN AN0 EVALUATION OF A DELAYED NEUTRON LEACHE 68PRR-059 NT I A L POL AROGP APPY/ A CELL DESIGN FOR MINIMIZING IR ERROR IN CONTROLLED PDTE 68PRR-083 UITS FOP DC POLAROGRAPHSI DESIGN OF TIME AVERAGING AND TIME DERIVATIVE CIRC 6BA-0 1- 10 INSTRUMENT FOR END POINT DETECTION IN BIP@TENTIOMETRIC TITRATIONS/ 68A-01-11 LOW LEVEL BETA DFTECTORI 68A-OB-OZF DERIVATIVE GAS CtROMPTCCWAPHY ( GAS CHROMbTOGRAPHIC 3ETECTDR SPECIFIC FCR SILICON If 68A-02-01H GANO PHOSPHORIJS POLYMERS / 5 FIJ9FURYL FURFURYL ALCOHOL / @FUTERD Dl METHYL SULFOXIDF / HEXA METHYL PHDSPHO 680-11-04 NEW DEVFLDPMENTS IN PCTIVATIDN ANALYSIS/ 68PRR-114 RECENT DEVFLGPMENTS IN ACTIVATION ANALYSIS/ 68PRR-129 AL TUBES/ DEVICE FOR SAMPLING GASES CONTAINED IN SEALED MET 68A-02-D1C ONS/ DEVICE FOR THE UNATTENDED CONCENTRATION OF SOLUTI 68A-02-D5C ENE 3717 OlONE I 2 0FTA METCVL ESTRA 4 EVE 3117 OIONE / DI BROMO FLUORENE / TRUXENE / UREA / VARCUM / PAP 6 88- 11- 04 RI METHYL PHOSPHATE / El METI-YL BUTYL PHOSPHATE / METHYL 01 BUTYL PHOSPHATE I/ DETERMINATION OF THF METHYL bBA-02-ClE DETFPMINATION IlF SILICON IN CURIUM OXIDE ( DI CURIUM-2L4 TRI OXIOE )I 68A-0 5-0 5 ,5 HEPT4NE nIChE )I PREPARATION AND ANALYSIS OF THE BETA DI KETONES OF THE LANTHANIDES AND ACTINIDES ( AHE 68A-02-076 STERS Dc RUTYL PhDSPHORIC ACIOS ( TDI METHYL PHOSPHATC / DI METHYL auTYL PHOSPHATE METHYL DI BUTYL PHDSP 68A-02-D1E POLARDGRAPt'Y 'IF ZIRCONIUM IN ACETONITRILE AND DI METHYL SULFOXIDE/ 684-01-07 QUANTITATIVE FLECTROGEPOSITICN OF ACTINICES FROM DI METHYL SULFOXIDE/ 68A-08-020 SPHORLIS FDLYMEhS / 5 FURFUPYL ALCOHOL / DEUTERO DI YETHYL SULFOXIDE / HEXA METHYL PHOSPHORIC TRI 686-11-04 UM ALLOY / NICKEL-61 - IRON ALLllY / POTASSIUM HEXA CYANO DI NICKELATE(I1 / POTASSIUM NICKEL(IV1 PARA PEP I 68A-09 TERFEFENCFS TO WINKLER MFTHCC / DEAERATED WATER / CARBON 01 OXIDE I/ DEAERATION SYSTEMS ( DISSOLVED OXYGEN 6 OA- 02- 04C / POLAPOGRAPHY OF SULFUR DI OXlOE ( SULFITE I IN AQUEOUS HYDROFLUORIC ACID 68A-02-OBC R MAGNFTIC RESONhNCE SPECTRCMETRY ( CINNAPYLIOENINCENF / 01 PHENYL 0ENZO FULVENE I POLY METHYLENE POLY PHE 680-11-04 RMINATION OF CADMIUM IN PLUTONIUM ( AHMPNIUM PYRROLIDINE 01 THIO CARaAMATF I APDC 1 )I DETE 688-05-048 POLY TETRA FLUOR0 ETWYLFNE ( TEFLON ) AS AN ADSORBENT ( DI 2 ETHYL HEXYL CRThC PHOSPHORIC ACID / HDEHP / 68A-O2-@2B 0 ION EXCHANGERS I/ FECLAIMING AMINO PCIOS - CARBON-14 ( 01 2 ETHYL HEXYL CPTHD PVDSPHDRIC ACID / HDEHP / 68A-04-016 FLUORIDF SALTS )I CONTAINERS FOR MOLTEN FLUORIDE SALTS ( DIAMOND WINDOWED CELL FDK SPFCTRDPHOTOMETRIC MEAS 68A-03-02F PDGRAPHYI COVTRflLLED POTENTIAL DIFFERENTIAL CC POLAROGRAPHY V. SUBTRACTIVE POLA 68PRR-033 ES PROGRAM I/ PCLAROGRAPHIC SURVEY UF BIDCHEMICALS ( DIFFERENTIAL DC POLAROGRAPHY / BODY FLUIDS ANALYS 68A-01-08 RECENT ADVANCES IN DIFFERENTIAL PCLAPCGRAPHYl 68PRR-119 RESEARCh ASSISTANCE IN ELECTRON MICROSCOPY AN0 ELECTRON DIFFRACTI@N/ 686-07-01 COMPUTER ASSISTED ANALYTICAL CHEMISTRY ( DIGITAL COMPUTER / LOGIC MODULES )I 68A-01-20 .E. / CNSEMRLF AVERAGING I/ ANALYTICAL APFLICATIONS OF A DIGITAL INSTRUMENT COMPUTER SYSTEM ( POLAROGRAPHY 68A-01-21 USE FOR DIGITAL POLAROGRAPHY/ 6BA-01-210 ON OF SUFNANCMOLE QUANTITIES OF L AMINO ACIDS EY ISDTDPF OILUTICN - AMINO ACYLATION/ DETEPMINATI 68A-04-01L NUCLEIC ACIr eASESv NUCLEOSIDES, AND NUCLEOTIDES @Y TWO DIMENSIONAL THIN LAYER CHROMATOGRAPHY ON POLY ETH 68PRR-027 ON FLECTRON VOLT NEUTRON IRRADIATIONS/ THREE DIMENSIgNALLY ROTATING SAMPLE HOLDER FOR 14-MILL1 68PRR-012 GERMANIUM - LITHIUM 01 CDE GPYM A S PECT RCMETRY SY STFMI 684-08-04E FLUORQ ACFTYL ACFTONE / 2rZrtr6 TETRA YETHYL 315 HFPTANE DIONE I/ PFEPARATION AN0 ANALYSIS OF THE BETA DI 684-02-075 ESTRA zi ENE 2-17 OICNF / 2 BETA METHYL ESTRA 4 ENE 3.17 DICNE / Dl BROMO FLUORENE / TRUXENE / UREA / VARC 680-1 1- 04 19 NnR TFSTO LOLACTONE / 2 ALPHA METHYL ESTRA 4 ENE 3.17 DlDNE / 2 BETA METFYL ESTRA 4 ENE 3,17 DIONE I DI 688-11-04 FLOW ANALYZER/ AN AUTOMATIC SAMPLER FOR D@TAINING DISCRETC SAMFLES FRCM THE OUTPUT OF A CONTINUOUS 68PRR-021 PLUTONIUM. NEPTUNIUM7 A'iC AYERICIUM ( FqTATING PLATlFlUM DISK ELECTRDCE / ROTATING PYROLYTIC GRAPHITF ELEC 68A-02-070 RANSFER RIB0 NVCLEIC ACIDS / TRANSFER QNA / FILTEP PPPER DISK TECHNIQUE )I INSTRUYENTATION FOR ANALYTICAL 68A-01-19 RIB0 FlUCLFlC ACID/ A SEMIAUTOMATED FILTE9 PAPER DISK TECHNIQUE FOR THE DETERMINITION OF TRANSFER 68PRR-003 ORIDE - RERYLLIUP FLUORIDE - ZIRCONIUM FLUORIDE AT 53OCI DISPROPORTIONATION OF ELECTROCHEMICALLY GENERATED 686-03-02A ORIDE - EERYLLIUM FLUCRIDE - ZIRCONIUM FLUORIDE AT 5DOCI DISPRDPORTICNATION OF ELECTROCWEMICALLY GENERATED 68PRR-CZ3 ORIDE - BERYLLIUM FLUORIDE - ZIRCONIUM FLUORIDF AT 500CI DISPROPORTIONATION OF ELECTROCHEMICALLY GENERATED 60PRR-109 D URANIU~(VI1IN MOLTEN LITHIUM TETRA FLVflRG BERYLLATE ( DISPROPORTIONATICN OF URANIUM(IV1 IN MOLTEN LITHI 688-03-D2E ROXY IS0 BUTYRIC ACIC / BERKELIUY-249 / CHRflMATDGRAPHY I DISSDLUTICN I FUSION / ION EXCHANGE / OXYGEN - TO 688-12-01 / POTASSIUM CtLDRIOE / flXYGEN / PYCNOMETER / SEALED TUBE DISSDLUTICN / THORIUM / URANIUM NITRIDE )I GENERA 688-12-02 EAERATED WATER / CARRON 01 OXIDE I/ DFAFRATION SYSTEMS ( DISSOLVED OXYGEN / SALINE WATER / INTERFERENCES T 684-02-D4C MODIFIED WILLPRD - WINTER OISTILLATION METHCD FOR FLUORIDE/ 688-1 C-13 F FLUORIDE/ RAPID OISTILLATION SEPARATION OF MICROGRAM QUANTITIES 0 68PRR-018 NTIAL DC POLARCGRAPH AND ORNL MODEL-Q-2"42 POLAROGRAPHIC DROP TIME CONTROLLER/ DRNL MODEL-Q-2792 CONTROLLE 68A-01-09 POLAROGPAPHIC DROP TIME COVTROLLER / MODEL-Q-2942f 68PRR-049 1 POLAR HYDROFLUORIC ACID WITH A VERTICAL ORIFICE TEFLCN DROPPING MERCURY ELECTRODE/ RAPID POLAROGRAPHY OF 688-02-088 POLAROGRAPHIC STUDIES WITH THE TEFLON DROPPING MERCURY ELECTRODE I D.M.E. I/ 686-02-08 )I APPbRI'US FCP PRECISE CCNTROL OF MFRCURY FLOW RITE DF DROPPING MERCURY ELECTRODES ( D.H.E. j I FIRST DE 6 8A- 01- C4 TRACE ELEMENTS IN DRUGS/ 68A-08-01E 2950 )I MOOIFlCATlON OF DUAL SET PGINT VOLTAGE COMPARATOR ( ORNL MOOEL-P- 681-01-15 E If DETERMINATION OF TRACES OF RAOE EARTH ELEMENTS IN BISMUTH ( CARRIER FREE PROCEOUR 68A-05-04A ACTIVITIES RELATED TO EDUCATIONAL INSTITUTIONS/ 6 80 ACTIVITIES RELATED T@ EDUCATIONAL INSTITUTIONS/ 680-14 SEPAPPTION OF CALIFORNIUM ( EINSTEINIUM I/ 6BA-02-D7F CE OF POLAROGPAPHSl ELECTRICAL AN0 ELECTRECHEMICAL TESTS OF PERFORMAN 68A-01-05 OPERATIONAL AMPLIFIER SYSTEMS IN ELECTROANALYTICAL CHEMISTRY AT ORNL/ 68PRR-IO1 ELECTROANALYTICAL RFSEARCH AT ORNLl 68PRR-093 C GRAPHITE AND PLATINUM METAL ELECTQDDES I/ SIMULTANEOUS ELECTROCHEMICAL ANC SPECTROPHOTOMETRIC STUDY OF S 68A-03-021 ITHIUM FLUORIDE - SODIUM FLUDRIOE - POTASSIUM FLUORIDE / ELECTRDCHEKICAL GENERATION AN0 SPECTROPHOTOMETRIC 68A-03-021 0 MOLE PERCENT I EVICENCE FOR ADSORPTION OF URANIUM(IVII ELECTROCHEMICAL REOUCTION OF URANIUM( IVI IN MOLTE 68PRR-CZ2 PHSf ELECTRICAL AN0 ELECTRECHEMICAL TESTS OF PERFORMANCE OF POLARDGRA 68A-01-05 RIDE - ZIRCONIUM FLUORIDE AT 5OOCI OISPROPCRTIONATIDN OF ELECTROCHEMICALLY GENERATED URANIUM(V) IN MOLTEN 686-03-024, RIDE - 7IPCONIUM FLUORIDE AT F.COC/ DISPRDPCRTlONATICh CF ELECTROCHEMICALLY GENERATED URANIUM(V) IN MOLTEN 68PRR-023 RIDE - ZIRCONIUM FLUORIDE AT 500CI OISPROPORTIONATION OF ELECTROCHEMICALLY GENERATED URANIUM(V) IN MOLTEN 68PRR-109 OPHDTOMETRIC STUGY OF SOLUTES IN MOLTEN FLUORIDE SALTS ( ELECTROCHEPISTRY OF TbNTALUR IN MOLTEN LITHIUM FL 68A-03-CZI N EVALUATION OF THE PERFORMANCE OF THE NITRATE SELECTIVE ELECTRODE/ A 68PRR-026 RIC ACID WITH A VEPTICAL ORIFICE TEFLON CROPPING MERCURY ELECTRODE/ RAPID POLAROGRAPHY OF URANIUM IN 1 MOL 684-02-C88 PERFORMANCE OF ION SELECTIVE ELECTRODES ( ORION SULFIDE ELECTRODE I/ EVALUATION OF THE 608-02-09 NG PLATINUM DISK ELECTRODE / ROTATING PYRDLYTIC GRAPHITE ELECTRODE )I VDLTAMPETRIC STUDIES OF PLUTONIUM. N 68A-02-C70 ONIUM, NEPTUNIUM, AN0 AMERICIUM ( ROTATING PLATINUM DISK ELECTRODE / ROTATING PYROLYTIC GRAPHITE ELECTRODE 688-02-070 POLAROGRAPHIC STUDIES WIT+ THE TEFLON DROPPING MERCURY ELECTRODE ( O.M.E. I/ 68A-02-00 RCE ( EMF I MEASUREMENTS IN MOLTEN FLUORIDES I REFERENCE ELECTRCDE FOR MOLTEN FLUORIDE SALTS )I ELECTRDMOT 68A-03-OZC N OF SIMPLE, REVFRSIBLE, DVERLAPPING WAVES IN STATIONARY ELECTRODE VDLTAHMETPY/ ON THE SEPARATION OF HALF- 688-01-14 N OF SIMPLE, REVERSIBLE, DVERLAPPING WbVES IN STATIONARY ELECTRODE VOLTAMYETRY/ ON THE SEPARATION OF HALF- 68PRR-025 THIN FILM MERCURY ELECTRODE VOLTAMMETRY OF BISMUTH/ 680-10-10 FOXID€/ QUANTITATIVE ELECTRCDEFOSITION OF ACTINIDES FROM DI METHYL SUL 6 BA-oe-oz o PERFORMANCE Tt-ARACTERISTICS OF ION SELECTIVE ELECTRODES/ 68PRR-120 ON VCLTAYMETRY AT PYRDLYTIC CRAPHITE AND PLATINUM METAL ELECTRODES )I SIMULTANEOUS ELECTROCHEMICAL AND SP 68A-03-021 126

PRECISE CONTROL OF MERCURY FLOW QAT€ OF DROPPING MCRCURY ELECTRODES I O.M.E. I I FIRST DERIVATIVE POLAROGR 68~-01-04 Q EVALUATION OF ThE PEQFCRYANCE CF ION SELECTIVE ELECTRODES I ORION SULFIDE ELECTRCllE I/ 686-02-09 QEMOVAL OF PHOSPHATE I ELECTROOIALYSIS I/ 68A-05-038 NEW METHOD I ELECTROOIALYSIS I/ 6PA-05-058 PIOES I REFERENCE ELECTRODE FOR MOLTEN FLUORIOE SALTS I/ ELECTROMCTIVF FORCE I EMF I MEASUREYEYTS IN MOLTF 68A-03-02C SOURCES OF CONTAMINATION DURING ELECTRON EEAM M€LTING/ 6 8P R R- C5 7 SOLRCES OF CONThMINATION DURING ELFCTRGN BEAM MELTING/ 6EPRR-O8@ RESE4RCH ASSISTANCE IY ELECTROY MICliCSCOPY AN0 ELECTRON DIFFPACTION/ 686-07-01 ON AN0 FAST NEUTRON ACTIVATION ANALYSIS AT THE OAK RIDGE ELECTRON LINFAR ACCELERATOR ( ORELA I/ PHOT t8A-06-018 OPTICAL AND ELECTRON MICROSCOPY/ 68A-07 RESEARCH ASSISTANCE IN ELECTROh YICRCSCOPY ANC ELFCTRON DIFFRACTION/ 68A-07-01 ELECTRON MICROSCOPY OF RADIOACTIVE MATER IALSl 68A-07-02 HREE DIMENSIONALLY RCTATING SAMPLE HOLDER FOR 14-MILLION ELECTRCN VOLT NEUTRCN IRRACIATIONSI T 6EPFQ-C12 ELECTRONIC INSTRUMFNTATIPNI 68PRR-094 GEL ELFCTROPHORFSIS CF PROTEINS/ 688-04-03F GEL ELECTROPHORESIS OF RIBO NUCLEIC ACID I RNA I/ 68A-04-01J FLUORIOE AT FPST SCAN RATES AND SHORT TRANSITION TIMFSl ELECTRCPEOUCTI3Y OF URANIUMIIVI IN M7LTEN LITHIUM 68PRR-10 8 OOIFICATION AND INSTbLLATICN OF PERKIN - ELMER YODEL-240 ELEVENTAL ANALYZER IN A GLOVE BOX I CARBON / HYO? 68A-02-07E NEh TITRANT DELIVERY UNIT AVO tLEVATOR/ 6EA-01-03A CLEbR TECHNOLOCYl SYNOPSIS '3F ELEVFNTH CCNFERENCE CN ANALYTICAL CHEMISTRY IN NU 68PRR-C32 / NITROGEN I/ MOOIFICATION AN0 INSTALLITION OF PFRKIN - ELMER MODEL-240 ELEMENTAL ANALYZER IY A GLOVE BOX 6EA-02-07E TROOE FOR MOLTEN FLUORIOE SALTS I/ ELECTROMOTIVE FORCE I EYF I MEASUREMENTS IN MOLTEN FLUORIDES 1 REFERFNC 668-03-02C EMISSION SPECTROMETRY/ 688-11-02 GANIC SYSTEM/ LIQUID SCINTILLPTICN CCUNTING OF kEAK EETA EYITTERS IN CQUEOUS SOLUTION RY USE OF TRITON X-1 684-OE-02G LIQUID SCINTILLATION COUNTING OF WEAK RETA EYITTERS IN AQUEOUS SOLUTION USIVG TRITON X-lOO/ 6EPRR-045 AESORPTIOY SPECTROPHOTOMETRY OF ALPHA EYITTING MATERIALS/ 689-10-12 BEAM SPLITTER FOR USE IN CALIBRATING SPECTROGRAPHIC EMULSIONS/ 6RA-05-02 BEAM SPLITTER FOR USE IY CALIBRATING SPECTROGRAPHIC EMULSIONS/ 68PRR-089 SI INSTRUMENT FOR EN0 POINT DETECTION IV BIPOTENTIOMETRIC TITRATION 684-01-1 1 HA METHYL ESTRA 4 ENE 3.17 OIONE / 2 BETA METHYL ESTRA 4 ENE 3,17 DIONE / 01 BROMO FLUORENE / TRUXENE / UR 68E- 11-04 A METHYL 19 NOR TESTO LOLACTONE / 2 ALPHA METHYL ESTRA 4 ENE 3-17 OIONE / 2 @ETA METHYL ESTRA 4 ENE 3.17 0 688-11-04 NEW NUCLEAR DATA I GAMMA-RAY ENERGIES / THERMAL NEUTRON CROSS SECTIONS I/ 688-08-038 OF SENSITIVITIES, INTERFERFNCES, AN0 OPTIMUM BOMBAROING ENERGIES IN HELIUY-3 ACTIVATION ANALYSIS/ RAPID C 6EPRR-030 PHOTOVOLTAIC CONVERSION OF RADIOISOTOPE DECAY ENERGY/ 6BA-OB-026 NDUSTRY EXPECTS OF THE GRADUATE IN CHEMISTRY OR CHEMICAL ENGINEERIhG/ WHAT I 68PRR-090 , ITALY, SWITZERLAND, CERMANY, WEST GERMAYY, NORWAY, AND FYGLANO, SEPT.2-3DrlS67/ REPORT OF FOREIGN TRAVEL 68PRR-C47 TO FRANCE; ITALY. GERMANY, THE NETHERLANDS, AND HARWELL, ENGLAND, SEPT.~-~~,IO~~/REPORT OF FOKEIGN TRAVEL 68PRR-058 HERLANDS, ~u~Y-10-31.196RI REPORT OF FOREIGN TRAVEL TO ENGLAND, SWITZERLAND, ITALY, GERMBNY. AN0 THE NET 68PRR-071 / SIGNAL AVERPGING AUTCMATICN / CIRCUIT TESTS / O.M.E. / ENSEMBLE DVERAGING I/ ANALYTICAL APPLICATIONS OF 686-01-21 A CELL OESIGN FOR MINIMIZING IR ERPOR IN CONTROLLED POTEYTIAL POLAROGRAPHY/ 68PRR-083 METHYL 01 BUTYL PHOSPHATE I/ DETERMINATION OF THE METHYL ESTERS OF BUTYL PHOSPHORIC ACIDS I TRI YETHYL PHO 68A-02-01E / 2 ALPHA METHYL ESTRA 4 ENE 3.17 DIONE / 2 EETA MFTHYL ESTRA 4 ENE 3.17 DIONE / DI BROMO FLUORENE I TRUX 688- 11- 04 / 2 BETA YETHYL 19 NOR TESTO LOLACTONE / 2 ALPHA METHYL ESTRA 4 ENE 3-17 CICNE / 2 EETA METHYL ESTRA 4 EN 68E-ll-C4 PHORIC TRI AMICE I BARIUM PARA ETHYL BENZENE SULFONATF ESTROLOLACTONE I 2 EETA METHYL 19 NOR TESTO LnLAc 688-11-04 LFOXIOE / HEXA METHYL PHOSPHORIC TRI AMIDE / RARIUM PARA ETHYL RENZENE SULFONATF / ESTP9LOLACTVNE / 2 9FTA ORE-1 1-04 TETRA FLUORO ETHYLENE I TEFLCN I AS AN AOSORECNT I 01 2 ETHYL HEXYL CRTHO PhOSPHORIC ACID I HOEHP / LIQUI 681-02-028 EXCHANGERS I/ RFCLAIMING AMINO ACIDS - CARBON-14 I 01 2 ETHYL HEXYL CRTHO PHOSPHORIC ACID / HOEHP / LIQUI 68A-04-ClG AYER CHROYATOGRAPHY I MASS SPECTRUM OF POLY T'TRA FLUORO ETHYLENE / MASS SPECTRUM OF OOLY ETHYLENE IYINF - 6PA-02-02F CIO / HOEHP / LIQUID ION EXCHAYGERS )I POLY TFTRA FLUCRO ETHYLENE ( TEFLON I AS AN ADSdREENT I 01 2 ETHYL 68A-02-02E UM OF POLY TETRA rLuoRc ETHYLENE I MASS SPECTRIJM OF POLY ETHYLENE IMINE - CELLULOSE I MASS SDECTRUM OF SEP 68A-02-02F NSTITUENTS OF TRANSFER RIB0 NUCLEIC ACID I TRNA I I POLY ETHYLENE IMINE - CELLULOSE / NUCLEOSIDES / NUCLFO 688-02-02C DES BY TWO OIYENSIONAL THIN LAYEP CHROMATOGRAPHY ON POLY ETHYLENE IMINE CELLULOSE/ QESOLUTION OF COMPLEX Y 6RPPR-C27 I KETONES OF THE LANTHANIOES AN0 ACTINIOFS I AMERICIUM / FUROPIUM / HEXA FLUORD ACETYL ACETONE / 2,2.6,6 T 68A-02-07G ICCN AUTOANALYZER / hYCROPONIC BEDS / ALGAL NUTRIENTS 1) EUTROPHIC WATER SYSTEMS I PHOSPHATE / NITRATE / T 6EA-02-046 A FILL PFCOROING RADIATION EVENT MONITOR FOR PULSE9 X AND GAMMA RAOlATION/ 6BPRR-O1! 2 ETHYL YCXYL ORTHO PHOSPHORIC ACID / HOEHP / LIQUID ION EXCHANGERS I/ POLY TETRA FLUORO ETHYLENE I TEFLON 68A-02-028 2 ETHYL HEXYL ORTHO PHOSPHORIC ACIO / HOEHP / LIQUID ION EXCHANGERS I/ RECLAIMING AYINO ACIDS - CARBON-14 68A-04-01G AVIOLET BAN0 STRUCTUPE - SOME CONCLUSIONS CONCFRNING THE EXCITE0 STATE OF URANYL ICNl ABSORPTION CF THE UR 68PRR-OD8 ENGINEERING/ WHAT INDUSTRY EXPECTS OF THE GRADUATE IY CHEMISTRY OR CHEMICAL 68PRR-090 ION ANALYSIS/ EXPERIENCE AN0 FUTURE OUTLOOK ON HELIUM-3 ACTIVAT t8PRK-111 AROMATIC HYOROCAREONS~ ALKALOIDS, PHENOLS, AN0 ACIDS I/ EXPLCRATORY STUDIES ( GAS CHROYATOGPAPHY OF POLY 684-02-036 KAGES SUEMITTEC TO THE DIVISION OF TECHNICAL INFORMATION EXTENSION/ INFORMATION PAC 68A-C1-22 NUCLEAR METHODS FOR EXTRA TERRESTRIAL ANALYSIS/ 68PRR-116 RUTHENIUM RADIOPCTIVITY IN AQUEOUS SOLUTIONSr PYRIOINE EXTQACTICh - GAMMA COUNTING METHOD/ 68PRR-080 ATION OF AMERICIUM FRCM GTHER TQANSURANIUM ELEMENTS/ NCW EXTRACTION CHROMATCGRAPHIC METHOD FOR THE RAPID S 688- 1C-03 DETERMINATION BY BETA COUNTING/ CHROMATOGRAPHIC SOLVENT EXTRACTION ISOLATION OF BERKELIUM-249 FROM HIGHLY 6EB-10-02 DETERMINATION BY BETA CCUNTING/ CHROMATOGRAPHIC SOLVENT EXTRACTION ISOLATICN OF SERKELIUM-249 FROM HIGHLY 6EPRR-013 EXTRALABORATORY PROFESSIONAL ACTIVITIES/ 68E FOR HOMOGENEOUS PHOTON AN0 NEUTRON IRRAOIATION IN REMOTE FACILITIES OF UNEVEN FLUX/ AIR FLOATING SPHERE 68A-08-01 A ION OF TRANSFER RIBO NUCLEIC ACID I TRNA I/ A FRACTION4L FACTORIAL METHOD FOR OPTIMIZIYG CGNOITIONS FOR TH 6EA-04-01C VATIVES OF AMINO ACIDS I/ BIOMEOICAL APPLICATIONS I FREE FATTY ACIDS / AMINO ACIDS / PHENYL THIO HYDANTOIN 6EA-02-010 NT MONTHLY SUMMARY - NDV.rl967 / OEC.11967 / JAN.9196P / FEE., 1968 / MAR.91969 I APR.91968 / MAY,1968 / J 68PRR-060 REPORT OF FOREIGN TRAVEL TO AUSTRALIA, FEBS1-MAR.7,1968/ 68PRR-044 ORAU GRAOUATE FELLOWSHIP PROGRAM/ 680- 14-03 A THIN FILM MERCURY ELECTRODE VOLTAYMETRY OF BISMUTH/ 6 8 B- 1 0- 1 0 X AN0 GAMMA RADIATION/ A FILM RECORDING RADIATION EVENT 'IONITOR FOR PlJLSEO 68PRR-011 CHEMISTRY I TRPNSFER RIBO NUCLFIC ACIDS / TRANSFER RNA / FILTER PAPER DISK TECHNIQUE I/ INSTRUMENTATION FO 68A-01-19 OF TRANSFER RIBO NUCLEIC ACID/ A SEMIAUTOMATEO FILTER PAPER DISK TECHNIQUE FOR THE DETERMINATION 6EPRR-003 -9- 17 34 AN0 MOOEL-6 4- 3 171 / FILTER PHOTOMETERS, REMOTELY OPERATED, ORNL MOOEL 68PRQ-073 STUDIES OF ABSOLUTE FILTERS/ 688-07-016 RY FLOW RATE OF DROPPING MERCUQY ELECTRODES I D.M.E. I I FIRST DERIVATIVE POLAROGRAPHY I/ APPARATUS FOR PR 6EA-01-04 SUQFACE IONIZATION 111. THE FIRST IONIZATION POTENTIALS OF THE LANTHANIDFSl 68PRR-016 HERES/ FISSION PRODUCT RELEASE FROM QEACTOR FUEL MICROSP 68A-O8-C4F MEASUREMENT BY GERMANIUM - LITHIUM GAMMA SPECTROMETRY OF FISSION PRODUCTS DEPOSITED IN COMPONENTS OF THE Y 6 EA-08-04C / IN REACTOR PENETRATION 3F FISSION PRODUCTS INTO MSRE AND PYROLYTIC GRAPHITE 6 EA- 08- 040 . USE OF STATISTICAL TECHNIQUES IN FLAME PHOTCMETRYI 68A-01-18 OF A DIGITAL INSTRUMENT COYPUTER SYSTEM ( POLAROGRAPHY / FLAME PHOTCMETRY / SIGNAL AVERAGING AUTOi-iATION / 686-01-21 MODEL IX FLAME SPECTROPHOTOMETER/ 68A-01-17 N IRRAOIATION IN REMOTE FACILITIES OF UNEVEN FLUX/ AIR FLOATING SPHERE FCR FCMOGENEOUS PHOTON AND NFUTRO 68A-08-01A TAINING DISCRETE SAMPLES FROM THE OUTPUT OF A CONTINUOUS FLOW ANALYZER/ AN AUTOM~TIC SAMPLER FOR 03 64PRR-021 POLAROGRAPHY I/ APPARATUS FOR PRFCISE CONTROL OF MERCURY FLOW RATE CF DROPPING MERCURY ELECTRODES I D.Y.F. 688-01-04 E OF STEROIDS I/ STEROIDS I GELMAN ITLC-SA MEDIUM / BODY FLUIDS ANALYSES / FLUORESCEYCE OF STEROIDS / PHOS 68A-02-02E EY OF BIOCHEMICALS I DIFFERENTIAL DC POLAROGRAPHY / BODY FIUIOS ANALYSES PROGRAM I/ POLAROGRAPHIC SURV 68A-01-08 127

DIONE / 2 BETA METHYL ESTRA 4 ENE 3.17 DIDNE / 01 BROMO FLUORENE / TRUXENE / UREA / VARCUM / PAP1 / FURFU 688-1 1-04 TEROIOS I GELMAN ITLC-SA MEDIUM / BODY FLUIDS ANPLYSES I FLUORESCENCE OF STEROIOS / PHOSPHORESCENCE OF STE 684-02-02E ~~OOIFIEOWILLARO - WINTER OISTlLLITlON METHOD FOR FLUORIDE/ 688-10-1 3 R4PID OISTILLPTION SEPARATION OF MICROGRAM QUANTITIES OF FLUORIDE/ 68PRR-018 4 V7LTAMMETRIC METMOD FOR CLUORIOEf 68PRR-036 UDRO EERYLLATE 4ND IN LITHIUM FLUORIDE - bRANIUM(IVI-233 FLUORIDE )I DETERMINITION OF OXIDE IN MSRE SALTS 68A-03-014 ON OF UQANIUM(1V) IN MOLTEN LITHIUM FLUORICE - SERYLLIIJM FLUOPIDE I/ SPECTPAL STUDIES OF IIRANIUM(V1 AND UR 69A-03-DEE TE ( DISPPOPOPTICNATICN SF U*bNIbM(IV) IN MOLTEN LITHIUM FLIJDPIOF - BERYLLIIJM FLUORIDE I/ SPECTRAL STUDIE5 t8A-03-02E ELECTROCHEMICALLY GENERATED UP4VIUM(Vl IF1 MDLTFN LITHIIIM FLUORIDE - BERYLLIUM FLUORIOE - ZIRCONIUM FLUORIO 68A-03-02A E 41 5OOCI VCLTIMYETRY OF CHRCMIUM(II1 IN YOLTEN LITHIUL" FLUORIDE - BERYLLIUM FLUORIDE - ZIRCONIUM FLUORIO 6flA-03-028 FCTRCCHEYIC4L REOUCTION OF URANIUM( IVI IN MOLTEN LITHIUM FLUORIDE - BERYLLIUM FLUURIDE - ZIRCOi4IUY FLUORID 68PRR-022 ELECTPOCHEMICALLY GENERATED UQANIUM( VI IN MOLTEN LI THIIJM FLUORIDE - BERYLLIIJM FLUORIDE - ZIRC.ONIUM FLUORIn 6RPRR-023 TIMES/ ELECTROPEDUCTION OF URANIUM(1VI IN MULTEN LITHIU'I FLUORIDE - BERYLLIUM FLIJOPIDE - ZIRCONIUM FLUrRlD t 8PR R-1 0 8 ELECTPOCHEMICALLY GENEQbTEO URINIUMIVI IN YOLTEN LITHTIJM FLUORIDE - RERYLLIUY FLUORIOE - ZIRCONIUM FLUORIO 68PRR-109 / VOLTAMMETRIC STUDIES OF CHROMIUM(II1 IN MOLTEY LITHIUM FLUORIOE - PERYLLILJ3 FLUORIDE - ZIRCONIUM FLUORID 68PRR-110 OETERMINATION CF TRACES UF BISMUTH IN LITHIUM FLUORIDE - BERYLLIUM FLUORIDE MlXTURESf 6 PA-05- 04C TURES ON THE SPECTRUM OF URANIUM(4+1 IN MOLTEN BERYLLIUM FLUORIDE - LITHIUM FLUORIDE MIXTURES/ CONTAINMENT 68PRR-006 REMENT OF COPPERIIII IN MOLTEN LITHIUM FLUGRIDE - SODIUM FLUORIDE - POTASSIllM FLUOhIDE / EFFECT OF OXIDE A 68A-03-021 HEMISTRY OF TbNTALUM IN MCLTEN LITHIUM FLUCRlilE - SODIUM FLUORIDE - POTASSIUM FLUORIDE / ELECTROCHEMICAL G 68A-03-021 E SALTS ( ELECTROCHEMISTRY OF TANTALUM IN MOLTEN LITHIUM FLUORIDE - SODIU*I FLUORIDE - POTASSIUM FLUDRIDE / 68A-03-021 OPHOTOMETRIC YE4SUPEMENT OF COPPERIII) IN MOLTEN LITHIUM FLUORIDE - SODIUM FLUORIDE - POTASSIUM CLUORIOE / 684-03-021 DE / EFFECT OF OXIDE AND HYDROXIDE IMPURITIES IN LITHIUM FLUORIDE - SOOldM FLUCRIDE POT4SSIUM FLUORIDE MEL 686-03-021 F OXIDE IN LITHIUM TETRb FLUORO 8cQYLLATi 4NO IN LITHIUM FLUORIDE - URANIUM(IV1-233 FLUORIDE )I OETERMINAT 68A-03-01A ON OF URANIUM(IV1 IN MOLTEN LITHIUM FLUORIDE - SFRYLLIUM FLUORIDE - ZIRCOYIUV FLUORIDE ( 65.6-29.4-5.0 MOL 68PRR-022 ON OF URANIUM(IV1 IN YOLTEN LITHIUM FLUORIDE - EERYLLIIJM FLUORIDE - ZIPCONIUM FLUORIDE AT FAST SCAN RATES 68PRR-108 ERATED URAYIUM(V1 IY MOLTEN LITHIUM FLUORIDE - BERYLLIUM FLUORIDE - ZIRCONIUM FLUORIZE 41 5DOCI OISPROPORT 684-03-02A ERATEO URANIUM(V1 IN MOLTEN LITHIUM FLUORIDE - BERYLLIUM FLUORIDE - ZIPCONIUM FLUORIDE AT 500CI DISPROPORT 68PRR-023 ERATEC URAVIUM(V) IN MOLTEN LITHIUM FLUORIDE - BERYLLIUM FLUORIDE - ZIRCONIUM FLUORIDE AT 500CI OISPROPORT 6flPRR-109 Y OF CHRO~lUM(1IIIN MOLTEN LITHIUM FLUORIDE - BERYLLIUM FLUORIDE - ZIRCONIUM FLUORIGE AT 500C/ VOLTAMMETR 68A-03-029 S OF CHROMIUM(II1 IN YOLTEN LITHIUM FLUORIO5 - BERYLLIIIY FLUORIDE - ZIQCONIUM FLUORIDE AT 50OCI VOLTPMMETR 68PRR-110 IN MOLTEN LITHIUM FLUORIDE - SODIUM FLUORIDE - DOTASSIUM FLUORIDE / EFFECT OF OXIDE AND HYDROXIDE IMPURITI 684-03-021 IN MCILTEN LITHIUM FLUDRIOE - SODIUM FLUPlIOE - POTASSIUM FLUORIDE / ELECTROCHEMICAL GENERATION AND SPECTRO 686-03-021 ANALYSES LABORATORY ( BISIIUTC / BULK PEhSITY / CYANIDE / FLUORIDE / PPTASSIUM ChLDPIDE / OXYGE?I / PYCNOWFT 689-1 2-02 MOLTEN LITHIUM FLUOQIDE - BERYLLlUiY FLUORIDE - ZIRCONIUM FLUORIDE ( t5.6-29.4-5.0 MOLE PERCENT I EVIDENCE 68PRR-022 MOLTEN LITHIUM FLUORIDE - EERYLLIUM FLUORIDE - ZIRCONIUM FLUORIDE bT FAST SCbN RATES AND SHORT TRAMSITION 68PRR-108 SURFACE IONIZATION OF URANlUMllVl FLUORIDE bT VAPIOUS CXYGEN PRESSURES/ 6 8A- 0 6- 03A MOLTEN LITHIUM FLUORIDE - BERYLLIUM FLUORIDE - ZIP.CONIUM FLUORIDE AT 500C/ DISPROPORTIONATION OF ELECTROCH 684-03-026 MOLTEN LITHIUM FLUOPlOE - RERYLLIUM FLUORIDE - ZIRCONIUM FLUORIDE bT 500CI DISPROPORTIONATION OF ELECTROCH 68PRR-023 MOLTEN LITHIUM FLUORIDE - RERYLLIIJM FLUORIDE - ZIRCONIUM FLUORIDE AT 5OOCI DISPROPORTIONATION OF ELECTRCCH 68PRR-109 MOLTEN LITHIUM FLUORI'JE - BERYLLIUM FLUORIDE - ZIRCONIUM FLUORIDE AT 500CI VOLTAYMETRIC STUDIES OF CHRClMIU 68PRR-110 MOLTEN LITHIUM FLUORIDE - BERYLLIUM FLUORIDE - ZIRCCNIIIM FLUORIDE bT 5OOCI VOLTAMMETRY OF CHROMIUM( I1 I IN 684-03-028 OETERMIQ4TION OF FLUORIDE IN A MIXTURE OF MOLYBDEhUM CLUURIOES/ 683-1C-0t BSORPTION - THERMAL CCNOLCTIVITY MEbSIJQEMENT OF HYORDGEN FLUORIDE IN GASES I/ DFTERMINATION OF UR4NIUM(III 6PA-03-018 SPECTRUM OF MOLY3DENUM(IIII FLUORIDE IN LITHIUM TETR4 FLUORO BERYLLATEI 68A-03-02H FLUORIDE IN MSRE FUEL, PYROLYSIS METHOD/ 68PRR-CBl SPECTROPHOTOYETRIC STUDIFS CF SOLUTE SPECIES IN MOLTEN FLUORIDE MEDII/ 64PRR-124 PURITIES IN LITHIUM FLCORIDE - SODIUM FLUCRIDE POTASSIUM FLUORIOE MELTS ON VOLTAMMETRY 41 PYROLYTIC GRAPtiI 684-03-021 ION OF TRACES OF BISMUTH IN LITHIUM FLUORIDE - SFRYLLIUM FLUORIDE MIXTUQESI OETERMINAT 68A-05-04C UM OF URANIUMI4+1 IN MOLTEN BEQYLLIUM FLUDRIOE - LITHIUM FLUORIDE MIXTURES/ CONTAINMENT OF MDLTEN FLUORIDE 68PRR-006 Y DE AND HYOROXIDE IMPURITIES IN LIT!iIUM FLUORIDE - SODIUM FLUORIDE POTASSIUM FLUORIDE MELTS ON VOLTAMMETRY 68A-03-02 I ANALYTICAL METHODS FOR THE IN-LINE PNALYSIS OF MOLTEN FLUORIDE SALTS/ 68A-03-02 17 NICKEL(I1). CbSUMIUM(1Ilr AND CHQOMIUMIIIII IN MOLTEN FLUORIDE SILTS I/ AESORPTION SPECTRA OF SEVERAL 3 6EA-03-02G DOWED CELL FOR SPECTROPHOTOMETRIC YEASUREMENTS OF MOLTEN FLUORIDE SALTS I/ CONTlINERS FOR MOLTEN FLUORIDE 68A-03-OZF NTS IN MOLTEN FLUORICES ( REFE9ENCF ELECTRODF FCR MOLTEN FLUORIDE SALTS I/ ELECTXOMOTIVE FOPCE ( EMF I MEA 68A-03-02C EMENTS GF YOLTEN FLUORIDE SALTS I/ CONTPiNERS FOR MOLTEN FLUORIDE SALTS I DIAMOND dINDOdED CELL FOR SPECTR 68A-03-OZF EMICAL AN0 SPECTROPHOTCMETRIC STUDY OF SOLUTES IN MOLTEN FLUORIDE SPLTS ( ELECTROCHEMISTRY OF TANTALUM IN 684-03-021 ETHODl NIORIUM IN MIXTURES OF FLUORIDE SPLTS, SPECTROPHOTOMET!?IC THIO CY4NATE M 68PRR-082 PTION SPECTRA OF SEVERAL TRANSITION METAL 13NS IN MOLTEN FLUORIDE SOLUTION/ ABSOR 68PRR-123 ON SPECTRA OF SEVERAL 3D TRANSITION METAL IONS IN MOLTEN FLUORIDE SOLUTION I ABSORPTION SPECTRA OF IRONIII 681-03-02G OETERMINATION OF FLUORIOE IN A MIXTUPE OF MOLYROENUM FLUORIDES/ 688-10-06 TS I/ ELFCTROMCTIVE FORCF ( EMF I YEASUREMENTS IN MOLTEN FLUCRIDES ( REFERENCE ELECTRODE FOR MOLTEN FLUOR1 68A-03-02C ORIDE - LITHIUM FLUORIDE MIXTURES/ CDNTAINMEVT OF MOLTEN FLUORIDES IN SILIC4 I. EFFECTS OF TEMPERATURES 0 68PRR-006 N 4NALYSISI DETERMINATION OF FLUORINE IN FLUORSPbR @Y 14-YEV NEUTRON ACTIVbTIO b 86-0 8-0 5 9 IQUEl PROTON RE4CTION ANALYSIS FOR LITHIUM AND FLUORINE IN GRIPHITE. USING 4 SLIT SC4NNING TECHN 68PRR-046 PPOTON REPCTION OiTFRMINATlON OF LITHIUM AND FLUORINE Ih' MOLTEN SPLT REACTOR GRAPHITE/ 68A-08-048 LANTHANIOES AND ACTINIDES ( AYERICIUM I EUROPIUM / HEX4 FLUORO ACETYL ACETCNE / 2.29696 TETRA METHYL 3-5 68A-02-07G SPECTRUM OF MOLYBDENUM(III1 FLUOSIOE IN LITHIUM TETRA FLUORO BERYLLbTE/ 68A-03-02H ES OF URANIUM(V1 AND URANIUM(VI1 IN MOLTEN LITHIUM TETRA FLUORO BERYLLATE I DISPROPORTIONATION OF URANIUM( 68A-03-02E ROFLUORINPTION ( DETERMINATICN OF OXIDE IN LITHIVM TETRA FLUORG BERYLLATE AN0 IN LITHIUM FLUORIDE - URANIU 68A-03-D1A GRIVIMETRIC OETERMINATION OF TETRA FLUOR0 BORATE WITH NITRONI 688-10-05 THIN LPYER CI'RCMATOGRAPkY ( MBSS SPECTRUM OF POLY TETRA FLUORO ETHYLENE I MPSS SPECTRUH.OF POLY ETHYLENE 68A-02-CZF HORIC AGIO / HOEHP / LIQUID ION EXCHANGERS I/ POLY TETRA FLUOR0 ETHYLENE ( TEFLON I AS AN AOSORBENT I DI 2 684-02-028 DETERMINATION DF PER FLUOR0 METHYL CYCLD kEXANE IN METHANE/ 68A-02-0 1F FLUORCHETRIC OETERMINATION OF PHOSPHATE/ 68A-02-040 DETERMINATION OF FLUORINE IN FLUORSPAR BY 14-MEV YEUTRON ACTIVATION ANALYSIS/ 68A-08-058 N PND NEUTRON IRRADIATION IN REMOTE FACILITIES OF UNEVEN FLUX/ 41R FLOATING SPHERE FOR HOMOGENEOUS PHOTO 68A-08-016 RADIONUCLIOES IN HIGH FLUX ISOTOPE REdCTOR COOLANT WATER/ 68A-08-06H NCE ELECTRODE FOR MOLTEN FLUCRIDE SALTS I/ ELECTROMOTIVE FORCE I EMF I MEISUREMENTS IN MOLTEN FLUORIDES I 68A-03-02C REPORT OF FOREIGN TRAVEL TO 4USTRALIAr FEB.l-MPR.7r196BI 68PRR-044 GERMANY, NORWIY, ANC ENGLAND, SEPT.2-30r1?67/ REPORT OF FOREIGN TRAVEL TO CZECHOSLOVAKlAr ITALY, SWITZERL 68PRR-047 TRIA. GREECE, AUG.29-OCT.811S67/ REPORT OF FOREIGN TRAVEL TO CZECHOSLOVAKIA, YUGOSLAVIA. AUS 68PRR-043 RMANY, ANC THE NETt4ERLANOSI JULY-l0-31,1968/ REPORT OF FOREIGN TRAVEL TO ENGLAND, SWITZERLANOt ITALY, GE 68PRR-071 ERLANDS, AND hPRWELL, ENGLAND, SEPT.5-26,1967/ REPORT OF FOREIGN TRAVEL TO FRANCE, ITALYI GERMbNYt THE NET 68PRR-058 FORENSIC APPLICATION OF TRACE ELEMENTS IN HAIR/ 68PRR-002 OETERMINITIDN OF TRDNSFER RIB0 NUCLEIC PCIO ( TRNA I/ A FRACTIONAL FACTORIdL METHOD FOR OPTIMIZING CONOIT 68A-04-01C Y/ FRACTIONATION OF HUMAN URINE BY GEL CHROMATOGRAPH 68PRR-084 CHROMATOERAPPY / FRACTIONATION OF IJRINE BY GEL AN0 ANICN EXCHPNGE 68A-04-D3C OF URINE/ G4S CHROMATOGRAPHIC ANPLYSIS OF FRACTIONS FROM THE ANION EXCHANGE CHROMATOGRAPHY 684-04-030 I MISS SPECTROMETRY 0.F URINE COMPONENTS )I DESALTING OF FRACTIONS FROM THE ANION EXCHANGE CHROMATOGRAPHY 68A-04-03E A LL, ENGLANO, SEPT.5-2t119t7/ REPORT OF FOREIGN TRIVEL TO FRANCE, IT4LYt GERMANY, THE NETHERLANDS, AND HARM 68PRR-058 DERIVATIVES OF 4MINO ACIOS I/ BIOMEOICdL APPLIC4TIONS ( FREE FATTY ACIDS / AMINO ACIDS / PHENYL THIO HYOA 68A-02-010 ON OF TRICES OF RARE EIRTH ELEMENTS IN BISMUTH ( CARRIER FREE PRDCEOURF )/ DETERMINATI 684-05-04A PRECISE OETERMINATION OF URANIUM IN MSRE FUEL/ 686-10-14 ATION OF IJRANIUM( 111) IN RADICACTIVE MOLTFN SALT REACTOP FUEL/ A TRAN7PIPATION MFTYOO '02 THE OETFkMIN 68PRR-0@7 SES )I DETERMIMATION OF URANIUM(1II) IN RADIOACTIVE MSRE FUEL BY HYO3OGEN RECUCTION ( LPSORPTION - THEhMAL t RA-03-01 B / ANALYSIS OF PURGE CAS FROM IN REACTOR TESTS OF REACTOR FUFL ELEMENTS ( MCNOPOLE 600 RCSIPIJAL GAS ANALYZC 68A-O3-C3A FISSION PRnDUCT RELEASE FQCM RFACTOR FUEL MICRCSPHERCS/ 6PA-OQ-04F FLUORIDE IN M5RE FUEL, PYROLYSIS YETHOD/ 6PPRR-CBl ANCE SPECTROMFTPY I: CINNAMYLIOENINDENF / 01 PHEYYL BFNZO FULVENE / POLY METHYLENE POLY PHENYL IS0 CYANATF 688-11-04 ON OF VERTICPL OPIFICE RAPID TEFLON D.M.F. FOR CBTAINING FUNDAMENTAL POL APOGQ APH I r DATA/ CV4LUATI 58A-02-0eA Y METHYLENE POLY PHENYL IS0 CYANATE / FURFIJRYL ALCOHOL / FIJPAN ALDEHYDE / OPGANO PHOSPHOPUS POLYMEFS / 5 F t RR-11-04 E / 01 BROMO FLUORENE / TRUXFNE / IJREA / UARCUM I PAPI / FURFURAL / HIPPURIC ACIC / CAPYOPHYLLENE / LIPI'IS 688-11-04 FURAN ALOEtYDF / OQGANO PkOSPHIRUS POLYMERS / C. FURFURYL FURFURYL ALCOHOL I OEUTERO DI MtTHYL SULFOXIDE I 68B-11-04 BENZO FULVENE I PnLY YETHYLENE POLY PHENYL ISO CYANATF I FURFURYL ALCOHOL / FURAN 4LDChYOE / GRGANO PHOSPH 683-11-04 LCOHOL / FURAN ALCEHYOE / ORCANO DHOSPHOPUS POLYMERS / 5 FUQFUHYL FURFURYL ALCOI-OI / DEUTERO 01 YETHYL SUL 6~e-11-04 IC ACID / BERKELIUM-249 / CHPCMATOGRAPHY / DISSOLUTION / FUSION / ION FXCHANGE / OXYCEH - TO - METAL PCTlO 689-12-01 EXPERIENCE AND FUTJRE OUTLOOK ON HEL'IJM-I ACTIVATION ANALYSIS/ 6RPRR-111 PUM OF SEDHADFX-G-75 / MASS SPECTRUM OF MFRCK SILICA GEL G / MASS SPECTRUM OF CZRNIUG PflDOllS GLASS 7?3< / 68A-O?-02F ADIOACTIVITY IN AQUFOUS SOLUTIONS. PYRIDINE EXTQACTION - GAMMA COUNTING MFTHODl PLITHENIU~~R 68PRR-080 FILM RECOROINC RACIATION EVENT MONITOR FOR PULSE0 X AN0 GAMMA RADIATICN/ 4 68PRR-011 IRON/ EFFECT OF SAMYA RACIATION ON SPECTROPHGTOMFTQIC METHDUS FnP 68A-OP-07F FFFFCT- __ IlN. ANALYTITAL PROCEOUQFSI CYLrQIMF PROOUCTION BY ZAMYA RAOIOLY5IS OF ACID CHLOPIDE SOLLITICbIS ANT: I h 8PP R-019 MPONENTS OF TtE MSQE/ MEASUREMENT BY GEPYPNIUW - LlTHlUY GAMMA SPFCTROPETRY CF FISSION PRODUCTS DEPOSITFD 68A-OD-04C GEQMANIUP - LITHIUM DIODE GAMMA SPECTROMFTRY SYSTEM/ 6PA-08-04E NS I/ NEW NUCLEAR DATA ( GAMMA-RAY ENFRGIES / THEPMAL hEUTROY CROSS SFrTICI 66A-OR-C3R GAMVA-RAY INTEIqSITIfS 1U THC OECAY OF BAFIUM-lli/ 68A-On-C3F V NEUTRON IRRACIATlONSl STANOARO GAM'4A-RAY SPECTR.1 OF THE FLENtNTS FllLLOWlNG 14-PF 68PRQ-121 LUTETIIJM-172 GOES TO YTTERBIUM-172/ INVESTIGATION OF GAMMA-RAYS IN THC CFCAY CHAIN HAFMIIJM-172 GOES TO 68PRR-115 R TESTS OF REPCTOR FUEL ELEMENTS f MONOPOLE 600 RESIDUAL GAS ANALYZER )I 4WALYSIS PF PUPGE GAS FQOM IN RFA 686-03-036 RATIVE.~ SAS CHRCMATOGRAPHY ( VA2IAN-AEROGRAPH PRFPARATIVE GAS CHROMATOGRAPH )I PR iP4 68C-07-01G E ANION EXCHANCE CHRCMATOCRAPHY OF URINFl GAS CHROMATOGRAPHIC ANALYSIS OF FRACTIONS FQOM Th b8A-04-030 I/ DERIVATIVE GAS CHROMATOGRAPHY ( GAS CHQOMATIGQAPHIC OETECT?R SPECIFIC FOR SILICON bF A-02-C 1H NSTITUENTS AND RFLATEC COf'POUNOSl CATALOG OF GAS CHROMATtlGkAPHlC RETENTI3;I.I 7ATA FOR URINARY CO h8PRR-037 GAS CHROMATOGRAPHY/ 686-92-01 A REMODELED LABORATORY FOR GAS CHROMATOGRPPHY/ ~~A-O~-OIB AQUEOUS INJECTION GAS CHROMATOGRAPHY/ 68A-02-046, SPECIFIC FOR SILICON I/ OFRIVAT1 VE GAS CHROMATOGRAPH? ( GAT CHQGMATDC9APHIC TFTFCTUR 638-02-01H GAS CHROMPTOGRAPH )I PREPARATIVE GAS CHQOMATOGELPHY ( VARIAN-AEROGRAPH PREDAPATIVE bE'A-02-OlG ,.~ PLKALOIDS. PHENOLS. ANP ACInS I/ EXPLOR4TOPY STUOIFS ( GAS CHROMATJGKAPHY OF POLY NlICLE2R AROHATIC HYDRO 6'IA-C2-C34 MONDPOLE.60C RESInU4L GAS ANALYZE9 )I ANALYSIS OF PURGE GAS FROM IN REACTOR TFSTS Ili PkACTGR FUEL CLEMFNT 6 8 A- 0 3 - Ct 3 A THERMAL CONDUCTIVITY MEASUREMENT OF HYDROGEN FLUORIDE IN GASFS )I DETERWINATION OF UQANIUMIIII) IN PAOIOAC 68A-03-GlB DEVICE FOP SAMPLING GASES CONTAINED IN SEALtD METAL TU9ESI 684-02-01C FRACTIONATION OF URINE BY GEL AND ANION EXCHAQGE CHRO*ATqGPAPHY/ 6 PA- 0 4- 0 3 C FRACTIONATION OF HUMAN URINE @Y GEL CHROMATOGRAPHY/ 66PRR-CB4 GEL FLECTROPHORFSIS OF PROTEIhlSl 6RA-04-03F GEL ELECTROPYORFSIS OF SIB0 fvUCLClC ACID I PkA I/ 6el-04-GlJ PECTRUY OF SEPPADEX-G-75 / MASS SPECTRUM OF MERCK SILICA GEL G I MASS SPECTRUM OF COPNIWG POQOUS GLASS 793 oBP-D2-02F CHNIOUF/ GEL PERMEATION CHKOMPTOGRAPHY AS A SEPAPATIONS TE 686-10-11C N OF-SIX CORTICOSTERCIDS BY THIN LAYER CHRCMATOGRAPHY ON GELYAN ITLC-SP MECIUYl SEPARATIO tPPRR-076 OF STEROIOS / PHOSPHORESCENCE OF STEROIDS I/ STEROIOS ( GELMAN ITLC-SA MECIUM / 80OV FLUIDS CNALYSES / FL 6@A-O7-D2F SPECTRUM OF COPNING POROUS GLASS 7935 / MASS SPECTRUM OF GELMAN ITLC-SA MECIUM / MASS SPECTRUM CIF ALUMINA 6RA-02-02F HDMOGEYEOUS PRECIPITATIONS USING PAOIOLYTICALLY GENERATED HYDROCHLPRIC ACID/ 6PPPR-103 LUORIOE PT 500C/ DISPROPORTIONATION OF ELECTROCHEMICALLY GENERATED URANIUMIV) IN MOLTEN LITHIUM CLUOGIOE - t8A-03-02A LlJORlDE AT 500C1 DISPROPORTIONATION OF ELECTROCHEMICALLY GENFRATEO URAhIUM(V) IN MCLTFN LITHIUY FLUORIDF - 68PRR-023 LUORIOE AT 50DCI OISPQOPORTIONATION OF ELECTROCHEMICALLY GENERATED URANIUM(V1 IN MOLTEh LITHIUM FLUORIDE - 6 BPRR- 109 - SOOIUM FLUORIDE - POTASSIUM FLUOPIDE / ELECTROCHFMICAL GENERATICN AND SPFCTROPHOTOMFTRIC MEASUREMENT OF 686-03-021 TREND IN ATCMIC POIJEQ GENERATICN AN0 URANIUM RESnUFCFS/ 68TR-02 14-MEV NEUTRON GENERATOR/ 681-08-05 -MEV NEUTRON ACTIVATION )I 14-MEV NEUTRON GENERATOR STUDICS I DETERMINATION OF UXYGEN PY 14 68P-OP-05A NFI. - lTRnN . . . - . GENERATOR TARGET OEVELOPYFNT OROGRAMl 68A-OR-05C LOW LEVEL RPCIATION COUNTING FACILITY FOR GEOCHEMICAL AND RETJRNED LUNAR SAMPLES/ 68A-08-02H ENTS/ GEOLOGICAL AGE DETERMINATIOY BY ISOTOPIC MEASURFM 68PQR-127 EM/ GERMANIUP - LITHIUM CIODE GAMMA SPECThOMETRY SYST 6 et- oe-04~ ;CTS DEPOSITED IN COMPONENTS OF THE MSRE/ MEASUREMEWT BY GERMANIUM - LITHIUM GPPMP

A

N STATIQMARY FLFCTFODE VOLTS3METRY/ ON THE SEPCRATION OF YALF-WAVE POTFNTIPLS WCQUIFEO FOR RESOLUTION OF S 684-01-14 N STAT1ONAF.Y ELECTROGE VOLTAMYETRY/ ON THE SEPARATION !3F HALF-WAVE POTENTIALS REQUIQED FOR RESOLUTIOY CiF S 6BPRR-025 N TRAVEL TO FRPNCE, ITALY, GERMANY, THE NETHERLANDS, AND qPRWELL, EKGLbNOt SEPT.5-26ilS67/ REPORT OF FORE1 68PRR-05e AN ACSrjrlBENT ( CI 2 ETHYL hEXYL CRTHO PHOSPHORIC ACID / HOEHP / LIQUID ION EXCHANGERS I/ POLY TETRA FLUOR 684-02-028 S - CARBOV-14 I CI 2 ETHYL HEXYL RRTHO PHOSPHORIC ACIO / HOEHP / LIQUID ION EXCHANGERS I/ RECLAIMING AMINO 6eA-04-01G INALYSIS OF 4SRE HELIUM FOR HYCROCAReONSl 684-03-010 INFLUENCE OF CHANNELING IN CCSTOKARY HELIUM-3 ACTIVATION ANALYS IS/ 68A-08-ClO EXPERIENCE 4W FUTURE OUTLCOK CN HE LIUM-3 ACTIVATION ANALYSIS/ 68PRR-111 ITIES. INTERFERENCES, AN3 OPTIMUX BUHRbRDING ENERGIES IN HELIUM-3 ACTIVATION ANALYSIS/ RAPID CALCULATION 0 68PRR-C30 ND BERYLLIUM/ INTERACTIONS 9F HELIUM-3 PARTICLES WITH EORON, iUlTPOGENt SODIUM A bPPRR-015 AMINO 4CID SEOUENCE CF MOUSE HEMOGLOBIN/ 6BA-04-C3H / HEXA ~LUOSOACETYL ACETONE / 2r27676 TETRA METHYL 3.5 HEPTANE OIONE I/ PREPAFATION AN0 ANALYSIS OF THE 68A-O2-C7G 44 - 4LUYINUM CLLUY / NICKEL-61 - IRON ALLOY / POTCSSIUM HEXA CYANO DI NICKELATE(I1 / PDTPSSIIJH NICKEL1 IVI 68A-09 F THE LANTHANICFS AND ACTINIDES ( AMERICIUM / FUROPIUM / YEXA FLUORC ACETYL ACETONE / 2~2,4~6TETPA METHYL 68A-02-07G URFURYL FURFUQVL ALCOI-DL / OECTERS DI METHYL SULFOXIDE / HEX4 METHYL PHOSPHORIC TRI WIDE / BARIUM PPRA ET 686-1 1-C4 OETERYIN4TION OF PER FLUORO METHYL CYCLO HEXANE IN METHANE/ 684-02-01F FLUORO ETHYLENE ( TEFLON I AS AN ADSORBENT I DI 2 ETHYL HEXYL CRTHC PHOSPHOPIC ACID I HOEHP / LIQUID ION 68A-02-028 NGEPS I/ PECLAIMING AMINO ACIDS - CARBON-14 I 01 2 ETHYL HEXYL CRTHG PHOSPHORIC ACID / HOEHP / LIQUID ION 68A-04-016 RbDIONUCLlDFS IN HIGH FLUX ISOTOPE REACTOR COOLAYT WATER/ 68A-08-06H TACTINIUM / TRAYSUR4NIUM ELEVENTS / URCI\!IA / ZIRCONIA )/ HIGH LEVEL ALPHI RPDIATION LABORATORY ( ALPHA HYD 686-12-01 L I/ INSTRUMFNTATION FOR THE HIGH P.AOIATION LEVFL bNbLYTIC4L LABORATORY ( HRLA 684-01-03 TITRATOR ( ORNL MPDEL-0-2564 I/ MODIFICATIONS TO THE HIGH SENSITIVITY CCNTROLLED POTENTIAL COULOMETRIC t8A-01-02 +?ODIFICATION OF THE ORNL MODEL-0-2564 HIGH SENSITIVITY CCULOMETRIC TITRBTOR/ 68PRR-048 544/ HIGH SENSITIVITY COULOMETRIC TITRATOR / MODEL-Q-2 48PRR-053 COULOMETRIC TITRATOR, CONTROLLED POTFNTIAL7 HIGH SENSITIVITYI ORYL MODEL-Q-256&/ 68PRR-077 0 FLLJORENE / TRUXEYE / UPEA / VARCUM / PAPI / FUP.FURAL / HIPPURIC ACIO / CARYOPHVLLENE / LIPIDS I/ NUCLEAR 688-11-04 I AT IONS/ TPREF CIMENSICNALLY PCTbTING SAMPLE HOLDER FOR 14-MILLION ELECTRRN VOLT NEUTRON IRRAO 68PRR-Cl2 DTF FACILITIES OF UNEVEN FLUX/ PIR FLOATING SPHFRE FOR YDMOGENECUS PVOTON AN0 NEUTRON IRRADIATION IN REM 68A-08-01A ENERATEO HYCPOCHL3RIC ACIOf HOM:3GENECUS PRECIPITATIONS USlNG RADIOLYTICALLY G 68PRR-103 GENERAL H@T ANALYSES LARORATORYl 688- 12-03 ICN FOR THE hIGh RADIATION LEVEL 4NALYTICbL LbRORATORY I HRL4L I/ INSTRUMENTAT 68A-01-03 THE DESIGN AND EVALUbTION OF A DELAYED NEUTRON LEACHED HULL MONITOR/ 48PRR-059 FRACTIONATION OF HUM4N URINE BY GEL CHROMATOGRAPHY/ 68PRR-C84 ERIVATIVES OF @MINO ACIllS / TRI MFTHYL SILYL PHENYL THIO HYCANTOIN DERIVATIVES OF AMINO ACIDS I/ BIOMEOICA 68A-02-010 LICATIONS I FREE FATTY PClDS / AKIYO ACIDS / PHENYL THIO HYCANTOIN DERIVATIVES CF AMINO ACIDS / TRI METHYL 68A-02-010 ANALYSIS OF MSRE HELIUM FOR HYDROCARBONS/ 686-03-010 RY STUDIFS ( GAS CHROMATCGRAPHV OF POLY NUCLEAR AROMATIC HYOROCARBONSI CLKALCIDS. PHENOLS, AN0 ACIDS I/ EX 68A-02-038 OPOGEMEOUS PRECIPITATIONS USING RADIOLYTICALLY GENERATED HYDROCHLORIC ACID/ H 6ePRR-103 LLEO DFHYDQATIDN I/ CONCENTRATING HYDROCHLORIC ACID ( HYOPOGEN CHLORIDE-36 / CONTRO 6BA-02-050 PflLARVGRAPHY OF SULFUC GI OXIDE I SULFITE I IN AQUEOUS tiYOROFLUGRIC ACID/ 684-02-C8C CURY ELFCTRODEI CAPIO PCLAPOGPAPHY OF UW4NIUM IU 1 HOLAR HYOROFLUOPIC AGIO WITH 4 VEQTICAL ORIFICE TEFLON 68A-02-086 -233 FLUORIDE I/ DETERMINATION OF OXIDt IN MSRE SALTS BY HYDROFLUORINPTION I DETEFfMINATICN OF OXIDE IN LIT 68A-03-01A R MOOEL-240 ELEMENTAL ANALYZEF IN A GLCVE BOX ( CARBON / HYDROGEN / NITROGEN I/ #ODIFICbTION AND INSTALLAT 68A-02-C7E CONCENTRATING HYDROCHLORIC PCIO I HYDROGEN CHLORIDE-36 / CONTROLLED DEHYDRATION I/ 68A-02-050 CTION I ABSCPPTION - THERMAL CCNOUCTIVITY MEASUREMENT OF HYDROGEN FLUORIDE IN GASES )I DETERMINATION OF UR 68A-03-018 ETERHINATION Oc UPANIUY(Il1l IN RADIOACTIVE MSRE FUEL BY HYDROGEN REDUCTION ( ABSOPPTION - THERMAL CONDUCT b8A-03-018 ANION EXCHPYGE CHRCMATOGRAPHY OF HYOQOLYZEC URINE/ 68A-04-038 SYSTEMS ( PHOSPHATE / NITRATE / TECHNICON AUTOANALYZER / HYOROPCNIC BEOS / PLGPL NUTRIENTS I/ EUTROPHIC WA 68A-02-048 DIUM FLUORIDE - POTASS1111” FLUORIDE / EFFECT OF OXIDE AN0 HYDROXIDE IMPURITIES IN LITHIUM FLUORIDE - SODIUM 68A-03-021 c LANTHANIDE HYDROXIDE SOLS/ 6BA-07-01A IRCONI4 I/ HIGF LEVEL ALPHA RPDIATION LABCRATORY I ALPHA HYDROXY IS0 BUTYRIC ACIO / eERKEL1IJM-249 / CHROMA 688-12-01 Y TETRA FLUORD ETHYLENE / MASS SPECTRUM OF POLY ETHYLENE IMINF - CELLULOSE / MASS SPECTRUM OF SEPHADEX-67 68A-02-02F S OF TRANSFER QIBO NUCLEIC bClD I ThNb I I POLY ETHYLENE IMINE - CELLULCSE / NUCLEOSJOES / NUCLEOTIDES / N 68A-02-02C 0 DIMENSIONAL THIN LAYER CHROMATOGRAPHY ON POLY ETHYLENE IMINE CELLULOSE/ RESOLUTlON OF COMPLEX MIXTURES 0 68PRR-027 IOE - POTASSIUM FLUORIDE / EFFECT OF OXIDE AN0 HYDROXIDE IMPURITIES IN LITHIUM FLUORIDE - SODIUM FLUORIDE 684-03-021 AN4LYTICAL METHODS FOR THE IN-LINE ANALYSIS OF MOLTEN FLUORIDE SALTS/ 68A-03-02 AL PROGRESS REPORTS 1964-1567/ CUMUL bTIVE INOEXES TO THE ANALYTICAL CHEMISTRY DIVISION ANNU b8PPR-C56 CUMULATIVE INDEXES TO THE ORNL MASTER ANALYTICAL MANUAL/ 68C-13-01 CHEMICAL FNGINCFRING/ WHAT INDUSTRY FXPECTS OF THE GRADUATE IN CHEMISTRY OR 68PRR-OS0 STABILITY OF SOME INERT METALS IN IRRACIATEO MINERAL ACIDS/ 6eA-OB-C70 DRMATION PACKAGFS SUBMITTED TO THE DIVISION OF TECHNICAL INFORMATION EXTENSION/ I NF 684-01-22 TECHNICAL INFORYATICN EXTENSION/ INFORYATION PACKAGES SUFYITTFO TO THE DIVISION @F 6BA-01-22 INFRARED SPECTROMETRY/ 688-11-03 HIN LAYFP CHRCMATOGRAPkY ( WICK-STICKS I/ INFRARED SPECTRCMETRY OF SOBSTANCES ISOLATE0 BY T 684- 0 2- 0 2G A QUE OUS INJECTION GAS CHROMATOGRAPHY/ 68A-02-04A 4LPHA PAOIATION CAMAGE IN INCRGANIC PHOSPHORS/ 68A-08-02C KELATE(1II / TFTRA KIS TRI PHENYL PHOSPHITE NICKEL101 I/ INORGANIC PREPARATIONS I AMMONIUM AZIDE / CALCIUM 681-09 E BOX ( CARBON / HYDROGEN / NITROGEN I/ MOOIFICATION AN0 INSTLLLATION OF PERKIN - ELMER MODEL-240 ELEMENTA 68A-02-07E ACTIVITIES RELATED TO EDUCLTIONAL INSTITUTIONS/ 6 80 PCTIVITIES RELATED TO EOUCATICNIL INSTITUTIONS/ 680-14 USE AS A LABORATORY TEST I NSTRUMENT/ 68A-01~21C SEYBLE 4VEQAGING I/ ANALYTICbL APPLICATIONS OF A DIGITAL INSTRUMENT COMPUTFR SYSTEM ( POLAROGRAPHY / FLAME 68A-01-21 ETRlC TITR4TIONSl INSTRUMENT FOR EN0 POINT DETECTION IN BIPOTENTIOM bBA-01-11 ANALYTICAL INSTRUME NTATI CNI t8A-01 INSTRUMENTATI GNI 68A-02-01A INSTRUMENT AT ICN/ 6 84- 0 7- 03 ELECTROYIC INSTRUMENT AT ION/ 68PRR-094 MODERN NUC.LEAR I NST RU ME NT AT I ON / 68PRR-118 INSTRUMENTATION ( CkRGMOSCAN I/ 68A-02-021 IC ACIDS / TRANSFER RNA / FILTER PAPER DISK TECHNIQUE I/ INSTRUMENTATIOY FOR ANALYTICAL BIOCHEMISTRY ( TRA 68A-01-19 YTICAL LAEORbTORY ( HQLAL I/ INSTRUMENTITIGN FOR THE HIGH RAOIATION LEVEL ANbL b8A-01-03 NEW INSTRUMENTS AN0 TECHNIQUES/ 68A-08-02 INTEGRATOR MODULFl 686-01-16 ATED CRAFT TRAINING/ VALIDITY OF SOME TESTS OF INTELLECTUEL A6lLlTY COR PREDICTING GRADES IN REL 6PPRR-005 GAMMh-RAY INTENSITIES IN THE DECAY OF BARIUM-133/ 68A-08-03F TROGENI SODIUM AN0 BERYLLIUM/ INTERACTIONS OF HELIUM-3 PARTICLES WITH 8OROhr NI 6PPRR-015 PLANNED USE WITH SPECIAL I NTERF 4C ES/ 6BA-01-218 bCTIVATION ANALYSIS INTERFERENCES/ 68PPR-105 / DEAERATION SYSTEMS I DISSOLVE0 OXYGEN I SALINE WATEP I INTERFERENCES TO WIYKLER HETPDO / DEAERATED WATER 68A-02-04C ACTIVATION ANALYSIS/ RAPID C4LCULATION OF SENSITIVITIES. INTERFERENCES, AN0 OPTIMUM BOMeAROING ENERGIES IN 68PRR-030 -57, MOLYEDENIJM-99 - TECHNETIII?,-99MI AN0 TECHNETIUM-99MI INTERLABORATDRY CCMPARISON OF MEASUREMENTS OF THE 68A-OR-C3 A ThERMDGRAVIYETRIC AbALYSIS OF THORIUM IOOATEl 688- 10-04 XA CYANO D1 NICKELATE(I1 / POTASSIUM NICKEL(IV1 PAPA PER IODATE 112 WATER / POTASSIUM TETRA CYANO NICKELAT 68A-09 130

PROOUCTION OF IODINE-123 FOR MEOICAL APPLICATIONS/ 696-08-06F PROCUCTION CF IODINE-123 MFCICAL APPL ICATIONSI CBPRR-017 8 FOE BARIUM-140 / SAMARIUM-151 / RHODIUM-ln3M / RUBIDIUM-84 / 1001NE-129 / IUOINE-130 I YTTRIIIM-91 / THULIUM-17 084-08-060 SAMARIUY-151 / RHODIUM-103M / RlISIOIUM-R4 / IOOINE-1?9 I IODINE-I30 / YTTRIUM-91 / THULIUM-170 I/ CHARQCTE bBA-OE-ObD SOME CONCLUSICNS CONCERNING THE EXCITEC STATE OF URANYL ION/ ABSORPTION OF THE URANYL ION IN PEA CHLORATE 6RPRR-COP RERKFLIUM-24‘3 / CHRPMATOGRAPPY / DISSOLUTION / FUSION / ION EXCHANGE / OXYGFN - TO - PETAL QAT10 / PLUTON 688-12-C1 01 2 EThYL HEXYL ORTHO PkOSPHllRIC ACID / WDEHP / LIUUIO ION EXCHANGEKS )I PQLY TETRA FLUOfiO ETHYLENE I TF 698- 02-028 CI 2 ETHYL HEXYL CRTHO PHOSPHllRIC ACID / HOEHP / LIOUID ION EXCHANGERS )I RECLAIYING APIh’fl LICIOS - CAQRON 6e4-0L-ClG HE EXCITE0 STATE OF VRANYL ICNl AESOFPTIUN OF THE URANYL ION IN PER CHLORATE YFCIA 111. RESOLUTION 3F THF 6PPP?-OCB PERFORMANC? CPARACTERISTICS OF ION SELECTIVE ELECTRODES/ tSFRR-120 E I/ EVALUATION OF THE PERFORMANCE OF ION SELECTIVE ELECT?OOES ( GRIUN SULfIOf ELECTROD 6RA-OS-CS -nc . THF, . . I- ANTUANI~FZ/...... - - . SIJRFACE IONIZATION 111. THE FIRST IONIZATION PCTFNTTALS 6ePRR-016 GEN PRESSURES/ SURFACE IONIZATION OF UPbhIUMlIV) FLUGRIOF AT VARICUS OXY 68C-06-C3d IONIZATION POTEWTIAL MEASUREMFQTSI tR4-OC-C3B SURFACF IONIZATInN Ill. THE FIRST IONIZATION POTENTIALS OF THE LANTHAAIDES/ 6hPRR-C1t 5URFACE IONIZATION STUDIES/ 68A-06-03 ABSCRPTION SPECTRA OF SEVERAL TRANSITION METAL IONS Ih CCLTEN FLUCRICE SOLUTION/ 68PRR-123 LTS )I A~SORPTIONSPFCTRA OF SEVERAL 30 TRANSITION METAL IONS IN MOLTEN FLUURIPE SOLUTION I CBSOQFTI9N SPE 6RA-03-OZG A CELL DESIGN FOR F1IhIMIZING IR ERROR IN CONTROLLFO POTENTIAL PCLAROGRAPYYI 6PPRR-OP3 ECT OF GAMMA RADIATION ON SPECTROPHOTOMETRIC METHODS FCR IRON/ EFF 68A-08-07F -73 TELLURIDE / NICKEL-64 - ALUMINUM ALLOY / NICKEL-61 - IRON ALLCY / POTASSIUM HFXb CYCNO DI hIICKEL4TFlI) 684-05 CHARACTEPIZATIDN OF ISOTOPE MATERIALS ( DECAY SCHEMES / IRflN-59 / 9ARIUM-140 / SAMARIUM-161 / RHOOIUH-103 68A-0e-060 ICNS IN HCLTEN FLUORICE SOLVTION ( ABSCRPTI@N SPECTRA OF IRDN(II17 hICKEL(II1, CHRCMIUM(II)l AN0 CHQOMIUM( t8A-03-C2G STABILITY OF SCMF INERT METbLS IN IRRAOIATEO MINERAL ACIDS/ 68b-08-070 AIR FLOATING SPtERE FOR tOM@GENEOUS PHOTON AND NEtJTRON IRRADIATICY IN REMCTE FACILITIES CF UNEVEN FLUX/ 68A-08-01A MMI-PAY SPECTRA OF THE ELElrEhTS FCLLDWING 14-MFV NFUTQON IRRAOIATIChSI STANDARC GA 6ePRR-121 ATING SAMPLE HCLOER FOR 14-MILLION ELECTRON VOLT NEUTRON IRRADIATIONS/ THREE DIMEYSICJNALLY ROT 58PRR-012 )/-HIGH LEVEL ALPHA RADIATION LAOORATORY I ALPHA HYDROXY IS0 BUTYRIC ACID / BERKELIUM-249 I CHROMATOGRAPHY 688-1 2-C1 E / 01 PHENYL BEN20 FULVFNF / POLY METHYLENE PllLY PHENYL IS0 CYANATE / FUQFURYL ALCOHCL / FURAH bLPFtYDF / 6Pe-ll-C4 ERMINATION OF SUBNANOPOLE QUANTITIES OF L AMIND ACIDS BY ISOTOPE OILUTION - AMINO ACYLATIOY/ GET 68A-04-01L NE-130 / YTTRIUM-91 / THULIUC-170 )I CHARACTERIZATION OF ISOTOPE MATERIALS ( DECAY SCHEMES I IRON-55 / EAR 6RA-08-06C RADIONUCLIDES IN HIGH FLUX ISOTOPE KEACTOR COOLANT dATtRI 6EA-08-nbH SPECIAL PNbLYTICAL ASSISTdNCE FOR ISOTOPES OEVELOfMENT CFNTER ACTIVITIES/ teA-CB-C6G COOPERATIVE ISOTOPES PROGRAM ( RADIOISOTOPES )I 664-08-06 CEDLOGICAL AGE DETFPMINATION BY ISOTOPIC MEASURFMENTS/ 68PRR-127

968l REPORT OF FOREIGN TRAVEL TO ENGLAND, SWITZERLANOI ITALY.~~ GERMANY, AN0 THE WETHE?LAYOS. JULY-10-31.1~. 68P44-071 AND. SEPT.5-26.1967/ REPORT OF FOREIGN TRAVEL TO FRANCE, ITALY; GERMANY; THE NETHERLANDS. ANh HARWELLt ENG 68PRR-C58 T.2-30,1?67/ REPORT OF FOREIGN TRAVEL TC CZECHOSLOVAKIA, ITALY, SWITZERLANOt GERYANY. WEST GERMANY, NORWAY 6 8P RR- 04 7 X CORTICOSTEROIDS BY THIN LAYER CHRUMATUGRAPHY ON GELMAN ITLC-SA MEDIUM/ SEoARATlON OF 51 bPPRR-076 ROIOS / PHOSPHORESCENCE OF STERDI9S )I STEROIDS ( GELMAN ITLC-SA MEDIUM / BODY FLUIDS ANPLYSES / FLUORFSCE 68A-02-O2E M OF CORNING POROUS GLASS 7535 / MPSS SPECTRIJY OF GELMAN ITLC-SA MECIUM / MASS SPECTRUM OF ALUMINA I/ MASS 6PA-07-OZF NO DEVELOPMENT MONTHLY SUMMARY - NOV..1967 I DEC.71967 I JAN..1968 / FEE., 1068 / MAR..lQ6+? / APR.91968 / 6PPRR-060 L QUALITY CONTROL REPORT- ANALYTICAL CHEMISTRY OIVISIONI JAN.-MAR.r1968/ STaTISTIC4 CSPRR-041 STRESS ANALYSIS IN TAPERED TRANSITION J@INTS IN REACTOR PRESSURE VESSEL/ 6e~il-01 .. 1963 / MAR.91968 / APR.rl568 / MAYv1968 / JUNE11963 / JULY.1968 / AUG.91968 / SEPl.rl9681 ANALYTICAL CH 68PPR-060 L QUALITY CONTRDL REPORT, ANALYTICAL CHEMISTRY DIVISION. JULY-SEPT-r1967/ STATIST1C.A 6RPRR-039 GI- ANO.. , SWIT7FRLAND.. - - - ITALY. GERMANY. AND THE NETHERLANOSr JULY-lO-31.1968/ REPORT OF FOREIGN TRAVEL TO EN 68PRF-C71 .,I968 1 FEB., 1968 / MAR.,l9t8 / APR.rI’366 / MAY71968 / JUNE11968 / JULYv196t? / 4UG.rla6e / SEPT.,1968/ A 6RPRR-Ob0 HFPTANF. . DInNF__ It PREPARATION AND ANALYSIS OF THE BETA 01 KETONES OF THE LANTHANIOES AN0 ACTINIDES ( AMF9IC 68A-02-07G EIC ACID ( TRNA )I KINETICS AMINO ACYLATION PF TRAQSFER RIB0 NUCL 68A-04-01F OF 5 112 WATER / POTASSIUM TETRA CYANO NICKELATF(I1) / TETRA KIS TRI PHENYL PhCSPHITE NICKEL(0) )I INORGANIC P 68A-OF ON/ CETERMINATION OF SUBNANOMOLE QUANTITIES OF L AMINO ACIDS BY ISGTOPE OILUTION - AMINO ACYLATI 686-04-01L DETERMINATION OF L ASDAPAGINASEl 688-04-01K THE ROLE OF THE LARGE NATIONAL RESEARCH LABORATORIES IN THE USA/ 68PRR-100 METtOD FOR SEPARATING MEMBERS OF ACTINIGE AN0 LANTHANIDE GROUPS/ 6 8P R R- 130 LANTHANIDE HYDROXICE SOLS/ ~~A-O~-OIA IONIZATION 111. THE FIRST ICNIZATION POTENTIALS OF THE LANTHANIDES/ SURFACE 6”PRR-016 / PREPARATION AN0 ANALYSIS OF THF BETA 01 KETONES OF THE LANTHANIOES ANr) ACTINIDES I AMFRICIUM / EUROPIUY 6eA-02-07G THIN LAYER CHROMATOGRAPHY/ 588-02-02 THIN LAYER CHRCMATOGRAPHYI 68A-C2-038 MINA )I MASS SPECTROMETRY OF SUBSTANCFS ISOLATFO BY THIN LAYER CHRCMATOGQAPHY ( MASS SPECTRUM OF POLY TETR 68A-02-02F INFhAREO SPECTROMETRY OF SUBSTANCES ISOLATED BY THIN LAYER CHROMATOGRAPHY I WICK-STICKS )I 684-02-02G SEPARATION OF SIX CORTICOSTEROIDS BY THIN LAYER CHRCMATOGRAPHY .GIN GELMAN ITCC-SA MEDIUM/ 68PRR-C76 ES, NUCLEOSIDES, AN0 NUCLEOTICES BY TWO DIMENSIONAL THIN LAYEP CHRCMATOGRAPHY flN POLY ETHYLENE IMINE CELLU 68PRR-027 THE DESIGN AN0 EVALUATIOY OF A DELAYED NEUTRON LEACHED HULL MONITCR/ 68PRR-C55 POTENTIAL COULOMETRIC DETERMINATION OF AMERICIUM ( HALF LIFE OF AMERICIUM-241 / HALF LIFE OF AYEQICIUH-24 68C-02-07A INATION OF AMERICIUM I HALF LIFE OF AMERICIUM-241 / HALF LIFE OF AMERICIUY-243 )I CONTROLLED POTENTIAL COU 688-02-078 TERMINAL NUCLEOSI9E ASSAY OF RIB0 NUCLEIC ACID BY LIGAND EXCHANGE CHRDMATOG2bPHYI 68A-0a-011 LIGAND EXCHANGE CHRCYAT9GRAPWYI 68A-04-C2 SEPARATION OF COMPOUNCS OF BIOLOGICAL INTEREST BY LIGAND EXCHANGE CHROMATOGRAPHY/ 68A-04-02B TERMINAL NUCLEOSIDE ASSAY OF RIRO NUCLEIC ACI’I BY LIGAND EXCHANGE CHROMATOGRAPHY/ 6RPRR-C09 / TERMINAL NUCLEOSIDES OF TRANSFER 9180 NUCLEIC ACIDS BY LIGAND EXCHANGF CHROMATOGRAPHY/ ASSAY OF 3 68PRR-C85 HELEX RESIN COLUMNS/ PRINCIPLES CF LIGAND EXCHANGF CHROMbTOSR4PHY ON COPPER LOAOEO C 68L\-04-02 A F RPOIATION - PrlECISIDN PHDTCMFTRY USING A RADIOISOTOPIC LIGHT SOURCFI ANALYTICAL APPLICATIONS OF THE SECO 68PRR-031 ST NEUTRON ACTIVATION ANALYSIS AT THE OAK PIOGE ELECTRON LINEAR ACCELERATOR I ORELA I/ PHOTON Ail0 FA 6 88-08-01 B RCUY / PAP1 / FURFURAL / PIPPURIC ACID / CARYOPHYLLENE / LIPIDS I/ NUCLEAR MAGNETIC RESONAYCE SPECTROYFTRY 688-1 1-C4 ROM MATER I ACETATE / AMBERLITE XA0-2 I/ EVALUATION OF A LIPOPHILIC ADSORPTION RFSIN FOR DESALTING AN0 REM 6 8A- 02- 05 8 RBENT ( 01 2 ETHYL HEXYL ORTHO PHOSPHORIC ACID / HOEHP / LIQUID ION EXCHANGtRS )I POLY TETRA FLUOR0 ETHYLF 684-02-028 ON-14 ( CI 2 ETHYL HEXYL CRTHO PHOSPHORIC ACID / HDEHP / LIQUID ICN EXCHANGERS )I RECLAI’4ING AMINO ACIDS - 68~-04-01~ THEORY AND PRACTICE TIF LIQUIO SCINTILLATICY COUNTING/ 68PRR-117 SFER RIP0 NUCLEIC ACIDS ( TRYA I/ COMPUTER PRXESSIhG OF LIQUID SCIhTILLATION COUNTING DATA IN THE ANALYSI 68A-04-01E US SOLUTION BY USE OF TPITON X-100 IN AN ORGANIC SYSTEM/ LIQUIO SCINTILLATICN COUNTING OF WEAK BETA EMITTE 68A-08-02G RS IN AQUEOUS SOLUTION USING TQITOY X-1001 LIQUID SCINTILLATICN COUNTIYG OF WEAK BETA EMITTF 68PRR-045 LITERATURE SURVEY/ 686- 10- 11A ANNING TECHNIQUE/ PROTON REACTION ANALYSIS FOR LITHIUM AN0 FLUORINE IN GRAPHITE, USING A SLIT SC 68PRR-046 ITEl PROTON REACTION DETERMINATION OF LITHIUM AND FLUORI~IE IN MOLTEN SALT FEACTOR GRAPH 68~-oe-o48 GERMANIUY - LITHIUM OIOOE GAMMA SPFCTROMETKY SYSTEM/ 686-08-C4E BERYLLATE ( OISPROPORTIONATION OF URANIUY(1VI IN MOLTEN LITHIUM FLUORIDE - BERYLLIUY FLUORIDE )I SPECTRAL 6eA-03-02E TION CF ELECTROCHEMICALLY GENERATE0 URANIUMIVI IN MOLTEN LITHIUM FLUORIDE - BERYLLIUM FtUORInE - ZIRC’3NIUY 6FA-03-O2A FLUORIDE AT 500CI VOLTAYMETRY OF CHROMIUM(I1I IN MOLTEN LITHIUM FLUORIDE - FERYLLIUM FLUORIDE - ZIRCONIUM 684-03-028 ([VI/ ELECTROCHEMICAL RECUCTICN OF URANIUM(1VI IN MOLTEN LITHIUM FLUORIDE - EERYLLIUM FLUORIDE - ZIRCONIUM 68PRR-C22 TION OF ELECTROCHEMICALLY CENERATED URANIUMIV) IN MOLTEN LITHIUM FLUORIDF - BERYLLIUM FLUORIDE - ZIRCONIUM 68FRR-027 NSITION TIMES/ ELECTRORECUCTION OF URANIUMIIV) IN MOLTEN LITHIUM FLUORIDE - PERYLLIUM FLUORIOF - ZIRCONIlJM 68PRR-108 13 1

TIOY OF ELECTFOCHEYICALLY GENERATED URANIUM(V1 IN MOLTEN LITt'IUM FLUORIDE - RERYLLIUM FLUORIDE - ZIRCONIUM 68PRR-109 AT 5@0C/ VOLTAMMETRIC STUOIES OF CHROMIU!4lII) IN MOLTEN LITH'IUV FLUORIDE - PERYLLIUM FLUORIDE - ZIQCONIUM 68PRR-110 DETERMINATION QF TRACES OF BISMUTH IN LITHIUM FLUORIDE - EERYLLIUM FLUORIOE MIXTURES/ 68A-05-04C FLIJORICF SALTS ( ELECTROCHECISTRY OF TANTALUM IN POLTFN LITHIUM FLUORIDE - SOOIUM FLUDPIOE - POTASSIUM FL 68A-03-CZI 0 SPECTROPHOTOMETFIC MEASUREMENT C1F COPPER1111 IN MOLTEN LITHIUM FLUOPIilF - SGOIUY FLUORIDE - PGTASSIUM FL 68A-03-021 M FLUORIDE / EFFECT OF OXIDE dV0 HYOROXIOE IMPURITIES IN LITHIIJM FLUORIOF - SOOIUM FLUCIAICE POTASSIUM FLU0 6PA-03-021 NATION OF OXIDE IN LITHIUM TETRA FLUORO BEPYLLATE AN0 IN LITHIUM FLUOkIOE - URCNIUMIIVI-233 FLUORIDE I/ OE 686-03-01A E SPECTRUY OF U~ANIUP(4tlIN MOLTEQ SFRYLLIUM FLUORIOE - LITHIUM FLUORIDE MIXTURES/ CONTAINMENT OF MOLTFN 68PRR-006 EO IN COMFONENTS OF TtE MSRFl WEAZUREMENT eY GERMANIUU - LITYIUM GAMMA SPFCTROMETRY OF FISSION PRODUCTS DE 68A-08-04C APPLICATIONS OF A BERYLLIUP klt130W GERMANIUM - LITHIUP SPECTROMETER SYSTEYl 684-08-03C SPECTRUM OF WOLY83ENUP(IIIl FLUDRIOF IN LITHIUM TETRA FLUORO PERYLLATEl 68A-C3-02H SPECTRAL STUCIES OF URLNIUMIVI AN0 UFANIUY(VI1 IN MOLTEN LITHIUM TETPA FLUORO EERYLLATE ( OISFROPOPTIONATI 686-03-02E E SALTS RY HYOPOFLUORINATION I OETERMINATION OF OXIDE IN LITHIUM TETRP FLUORO BERYLLATE AN0 IN LITHIUM FLU 68A-03-01A PRINCIPLES CF LIGANC EXCHANGE CHQOMPTOGPbPHY ON CCPPER LOADED CHELEX RESIN COLUMNS/ 68A-04-02A DRNL LOAYEESl 680- 14-04 PUTER ASSISTED PNALYTICAL CHE!4ISTPv I DIGITAL COMPUTER / LOGIC PCOULFS I/ COM 684-01-20 SULFONATE / ESTROLOLACTONE / 2 BET4 METHYL 19 NOR TESTO LOLACTONE / 2 ALPHA METHYL ESTilA 4 ENE 3917 DIONE 688- 11-04 POSSIBLE LOSS OF CESIUM DURING ASHING OF BONE/ 68A-05-07C LOW LEVEL BETA OETECTCRl 68A-Oe-CZF ICAL AN0 RETURNED LUNAR SAMPLES/ LOW LEVEL RAOIATICN COUVTTING FACILITY FOR GEOCHEM 68A-OB-OZH UNOS/ LOW RESOLUTION MASS SPECTR94ETRY OF ORGANIC COMPO 68A-06-02 PACIATION COUNTING FACILITY FOR GEOCHEIICAL AN0 RETURNED LUNAR SAMPLES/ LOW LEVEL 68A-08-OZH ION OF C-AMMA-RAYS IN TVE DECAY CHAIN HAFNIUM-172 GOES TD LUTETIUM-172 GOES TO YTTERBIUM-1721 INVESTIGAT CPPRR-115 ORNL SMOKING MACHINE/ 688-10-118 MACQOHOLECIJLAP SEPARATIONS PQOGRAM/ 6eA-04-Cl URAL / HIPPURIC ACID / CARYODHYLLENL / LIPIDS I/ NUCLELR MAGNETIC RESONANCE SPECTPOMETRY ( ClNNAMYLIOENINO ChE-11-04 MAINTENANCE OF THE CRNL MASTER ANALYTICAL MANUAL/ 68C-13-02 UTRON bCTIVATIGN ANALYSIS OF 6RAIN TISSUE FOR COPPER AN0 YANGANESEl NE 6861-08-C1F ORNL MASTER ANALYTICAL MANUAL/ 6RC ORNL MASTER ANALYTICAL MANUAL/ t8C-13 CUMULATIVE INDEXES TO THE ORNL MASTER ANALYTICAL MANUAL/ 68C-13-01 MAINTENANCE OF THE ORNL FASTER ANALYTICAL MANUAL/ 68C- 13-02 MMPRY - NQV..1967 / OEC.rl967 / JAN.tl9C.8 / FEE?., 1968 / MAR.vl968 / APR.vl968 / MPYT1968 / JUNE91968 / JU 68PRR-060 AMANITA TOXINS (GALERINA MARGINATA I/ 68A-02-020 NUCLEAR SPECTRCSCCPY IN THE NEUTRON OEFICIEYT MASS NUMPER BETWEEN 173-185 RFGIONl 6AA-08-030 MASS SPECTROMETRIC DATA REOUCTION/ 0 8A-06-04 MASS SPECTROMETRY/ hRA-Ob SPARK SOURCE MASS SPECTROHETRYI 68A-06-01 MASS SPECTROMETRY/ 686-1 1-01 TRANSURANIUM MASS SPECTROMETRY/ 68@-11-01A Leu RESOLUTIDN MASS SPECTROMETRY OF ORGANIC COMPOUNDS/ 688-06-02 P OF GELMAN ITLC-SA MEOIlJY / MASS SPFCTRUM OF ALUMINA I/ MASS SPECTROMETRY OF SUBSTANCES ISOLATED BY THIN 6RA-02-O2F CTIONS FROM TYF ANION FXCt'ANGE CHROMATOGRAPHY OF UPINE I MASS SPECTRDMETRY CF URINE COMPONENTS I/ OFSALTIN 6RA-04-03E MASS SPECTRCMETRY SE%VICES/ 68~-ii-oie US GLASS 7935 / MASS SPFCTRUP OF GELMAN ITLC-SA MEOIUM / MASS SPECTRUM OF ALUYINA 11 MASS SPECTROMETRY OF 68A-02-OZF OF SEPHAOEX-G-75 / MASS SPECTRUM OF MERCK SILICA GEL G / MASS SPECTRUM OF CORVING POROUS GLASS 7935 / MASS 68A-02-OZF ICA GEL G / MASS SFECTPUM OF CORNING POROUS GLASS 7935 / YASS SPECTRUM @F GELMAN ITLC-SA MEOIUM / MASS SPE 6PA-02-02F ENE IVINE - CELLULCSE / MASS SPECTQUM OF SEPHAOEX-G-75 / MASS SPECTRUM OF MERCK SILICA GEL G / MASS SPECTR 68A-02-02F TOGRAPHY I YASS ZPECTRUM OF POLY TETRA FLUORO ETHYLENE I MASS SPECTRUM OF POLY ETHYLENE IMINF - CFLLULOSE 684-02-02F n RY OF SUSSTPNCES ISOLATED 9Y THIV LAYEQ CHROMATOGRAPHY ( MASS SPECTRUM OF PCLY TETPA FLUCR3 ETMYLEhE / MAS 68A-02-OZF ENE I MASS SPFCTRUY GF PDLY ETI'YLFNE IMINE - CELLULCSE / YASS SPECTRUM OF SEPhACEX-G-75 / MASS SPFCTCUM OF 68A-02-02F ORNL MASTER ANALYTICbL MAYUALl 68C rRNL MASTER PNALYTICAL MANUAL/ 6RC-13 CUPULLTIVE INDEXES TO THE CRNL MASTER ANALYTICAL MANUAL/ 68C-13-01 MAINTENbNCE OF THE OFNL MASTER ANALYTICbL PANUALl 6@C-13-02 PHOTOMFTRIC STUOIES OF SOLUTE SPECIES IN MOLTEN FLUOPIOE ME01A/ SPFCTRO 68PRR-124 URANYL ION/ ASSOFPTION OF THE URANYL ION IN PER CHLORATE MFOIA 111. RESOLUTION OF THE ULTRAVIOLET BAN0 ST 6ePRR-008 PRODUCTION OF IODINE-123 FOR MEDICAL APRLICATInNSl 6PA-08-06F PRCOUCTION OF IODINE-123 FOR MEDICAL bPPL ICATIONS/ 68PRR-017 SOURCES OF CO4TAMINATION DUPING ELECTRON BEAM MELTING/ 68PRR-057 SOURCES OF CONTAMINATION DURING ELECTRON BEAM MELT INGl 68PRR-088 IN LITHIUM FLUORIDE - SOOIUM FLUORIDE POTASSIUM FLUOQIOF MELTS ON VOLTAMMETRY AT PYROLYTIC GRAPHITE AN0 PL 68A-03-021 4OVISOPY COMMITTEE MEMBERS AND CONSULTANTS/ 680-14-01 ?!FTHOO FOR SEPARATING MEMRERS OF ACTINIDE AN0 LANTi-ANIOE GROUPS/ 68PRR-130 LOSE / MASS SPECTRUM OF SEDHAOEX-G-75 / MASS SPECTRUM EF MERCK SILICA GEL G I %ASS SPECTRUM OF COKNING POR 684-02-02F YOROFLU091C ACID WITI' A VERTICAL PRIFICE TEFLOh OROPPIVG MERCURY ELECTROOEl RAPID POLAROGRAPHY OF URANIUM 68A-02-088 POLAROGPAPHIC STUOIES WITH THE TEFLON DROPPING MERCURY ELECTRODE I O.M.E. I/ 68A-02-08 THIN FILM YERCURY ELECTRODE VOLTAMMETRY OF BISMUTH/ 6138- io-ic TUS FOR PRECISE CONTROL OF MERCURY FLOW RATE OF DROPPING MERCURY ELECTRODES I O.M.E. 1 I FIRST OERIVATIVE 68A-01-04 IVATIVE POLAROGRAPHY )I APPARATUS FOR PRECISE CONTROL OF MERCURY FLOW RATE OF DROPPING MERCURY ELECTRODES 68A-01-04 MELTS ON VDLTAMMETRY AT PYROLYTIC GRAPHITE AN0 PLATINUM METAL ELECTRODES I/ SIMULTANEOUS ELECTROCHEMICAL 688-03-021 ABSORPTION SPECTRA OF SEVERAL TRAYSITION METAL IONS IN MOLTEN FLUORIDE SOLUTION/ 68PRR-123 IOE SALTS )I ABSORPTION SPECTRA OF SEVECAL 30 TRANSITION METAL IONS IN MOLTEN FLUORIDE SOLUTION I ABSORPTI 684-03-026 HY / @ISSOLUTION / FUSION / ION EXCHANGE / OXYGEN - TO - METAL RATIO / PLUTCNIA / / TRAYSURAN 688- 12-01 DEVICE FOR SAMDLING GASES CONTAINEO IN SEALED METAL TUBES/ 68A-02-01C STA8ILITY OF SOME INERT METALS IN IPQAOIATED MINEQAL ACIDS/ h8A-08-07G OETFRMINATION OF PER FLUORO YETHYL CYCLO HEXANE IN RETHANE/ 68A-02-01F METHIONINE TRNB I/ OETERYINATION OF HETHIONINE ACCEPTING TRANSFER RIB0 NUCLEIC ACID I ~~A-O~-OLB ION OF METHIONIVE ACCFPTING TPANSFER RIRO NUCLEIC ACID I METHIONINE TRNA I/ DETERMI NAT 68A-04-018 ANALYTICAL METHOOOL OGY/ 68A-02 RS OF BUTYL P~CSPHORIC ACIDS ( TRI METHYL PHOSPHATE I 01 METHYL BUTYL PHOSPHATE / METHYL 01 BUTYL PHOSPHAT 6EA-02-01E DETERMINATION OF PER FLU090 METHYL CYCLO HEXANE IN METHANE/ 68A-02-O1F IDS ( TRI METhYL PHOSPbATE IO1 METHYL BUTYL PHOSPHATE / METHYL 01 BUTYL RHCSPHATE 11 DETERMINATION OF THE 68A-02-01E HATE / METHYL 01 BUTYL PHOSPHATE I/ DETERMINATION OF THE METHYL ESTERS OF BUTYL PHOSPHORIC ACIDS ( TRI MET 68A-02-01E LACTONE / 2 ALPHA METi-YL ESTRA 4 ENE 3.17 OIONE I2BETA METHYL ESTRA 4 ENE 3917 OIONE / 01 BROMO FLUORENE 6 88-1 1- 04 LACTONE I 2 BETA METHYL 19 NOR TESTO LOLACTONE I2ALPHA METHYL ESTRA 4 €NE 3.17 OIONE / 2 BETA METHYL EST 688-11-04 ION OF THE METHYL ESTERS OF BUTYL PHOSPHORIC ACIDS I TRI METHYL PHOSRHPTE / 01 HETHYL BUTYL PHOSPHATE / ME 68A-02-01E YL FURFURYL ALC'JHOL / DEUTERO 01 METHYL SULFOXIDE I HEXA METHYL PHOSPHORIC TRI AMIDE / BARIUM PARA ETHYL B 688-1 1-04 / PHENYL THI'I HYDANTOIN DERIVATIVES OF AMINO ACIDS I TRI METHYL SILYL PHENYL THIO HYDANTOIN DERIVATIVES OF 68A-02-010 PGLAROCRAPHY OF ZIRCCNIUM IN ACETONITRILE AN0 01 METHYL SULFOXIDE/ 68A-01-07 WANTITATIVF ELECTROCEPOSITION OF ACTINIDES FROM 01 METHYL SULFOXIDE/ 68A-08-020 ORUS POLYMERS / 5 FURFURYL FURFURYL ALCOHOL / OEUTERO 01 METHYL SULFOXIDE / HEXA METHYL PHOSPHORIC TRI AMI bee-11-04 M PARA ETHYL BENZENE SULFONATE / ESTROLOLACTONE / 2 BFTA METHYL 19 NOR TESTO LOLACTONE / 2 ALPHA METHYL ES 688-11-04 / EUROPIUM / HEXA FLUORO ACETYL ACETONE / ZrZt6~6TETRA METHYL 375 HEPTANE CIONE I/ PREPLRATION AN0 ANALY 6SA-02-07G METHYLENE POLY PHENYL IS0 CYANATE / FlJRFURYL ALCO 686-11-04 Q RY ( CINNAMYLICENINOFNE I 01 PHENYL BENZO cULVENE / POLY MICRO TITRATILiN OF PLUTONIUff/ 684-02-07C QAPIO OISTILLATICN SEPARATION OF YICROGRAM QUbhTIlIES OF FLUOFIOEl 68PRR-018 PAQTICLE SIZE OISTRIBUTION OF PARTICLES FROM 10 TO 2000 MICRONS BY SEDIMENTATICN ANALYSIS/ 68PRR-007 OPTICAL AN0 ELECTRON YICQOSCOPY/ 688-07 RESEARCH ASSISTANCE IN ELECTRON MICPOSCOPY AND FLECTFON OIFFQArTION/ 68A-07-01 € L FCTR OM MICROSCOPY OF RAOIObCTIVE MATER IALS/ 6 R A- 0 7- 02 FISSION PRODUCT RELEASE FROM REACT09 FUEL MICROS PHE RES / 6PA-08-04F STABILITY OF SOME lNCRT MFTALS IN IRRAOIATEC MINERAL ACIDS/ 6PA-CB-07D OGRAPHYI A CELL DESIGN FOR MINIMIZING IR EPROQ IN CONTROLLED POTENTIAL 'OLAR 68PRR-083 ICAL PRECONC FNTR A T ION/ YISCELLANECUS TRICE CETERMINATIQNS INVOLVING ChEM 684-05-04 DETERMINATION OF FLUORIDE IN 4 MIXTURE OF MOLYROENUM FLUORIDES/ 688-1 0-06 NEh ORYL MOOEL-Q-l34?C PIPETTEsl 68A-01-038 AUTOMATIC POTENTIOMETRIC TITRATOR, VFLOCITY SERVO, ORNL MOOFL-Q-1728 AN0 MCOtL-Q-l728A/ 68PRR-C7@ IOMETRIC TITRATOR. VELOCITY SERVO, ORNL YOOFL-Q-1728 AN0 MODE L-Q-1728 A/ AUTOMAT IC POTENT 6PPRR-078 FILTER PPOTOMETERS, REMOTCLY CPERATEOv CRYL MODEL-8-1734 AN@ MCCFL-64-3 171I 68PRR-073 HTGH SENSITIVITY COULOMFTRIC TITRATOR / MODE L-Q-2564/ 6PPRR-053 C TITRATOR. CONTROLLED POTENTIAL, HIGH SENSITIVITYI ORNL MODEL-Q-2564/ CnuLom~~I 68PPR-077 ITIVITY CONTROLLED POTENTIAL COULOMETRIC TITRATOR ( ORNL MODEL-Q-2564 I/ '4UOIFICATIOhS TO THE HIGH SEN5 68A-OI-CZ R/ MOOIFICATION OF THE OQNL MODEL-8-2564 HIGH SCNSITIVITY COULOYETRIr TITRATr3 6 @ P P R- 04 8 CCYTRflLLFO POTENTIAL OC POLAROGRADH VOLTAMMETER / WOEL- Q-2 79 2 / 68PRH-050 NL MODEL-0-2942 POLARCGRAPHIC DROP TIME CONTROLLER/ ORNL MOOEL-Q-2792 CCNTROLLEO POTENTIAL OC POLdRCIGRAPH 688-01-09 POLARCGRAPHIC nR@P TIME CCNTROLLEF I MOCE L-Q-2942 I 68PRR-04a OOEL-9-7792 CONTROLLED POTENTIAL GC PGLARCGQAPH AN0 CRNL MODEL-Q-2942 POLARCGRAPHIC DRnP TIYE CONTROLLER/ h8A-01-09 MOOIFICATION OF DUAL SET POINT VOLTAGE COYPAPATOR ( ORNL MODEL-Q-2950 I I 6RA-01-15 ROGEN I/ MODIFICATION AN0 INSTALLATION OF PERKIN - ELMER MOOEL-240 ELEMEVTbL ANALYZFR 1'4 A GLOVE BOX ( CAR 6RE -02-C7E ER PHOTOYETFRS, REMOTELY OPERATED, ORNL MODEL-Q-1734 AN0 MODEL-64-3171/ FILT 68PrlR-073 MODERN NUCLEAR INSTRUMENTATION/ 68PRR-118 INTEGRATOR MOOU L E / 688-01-16 ASSISTED ANALYTICAL CHEMISTRY 1 DIGITAL COMPUTER / LOGIC MODULES I/ COMPUTER 686-01-20 NG MEPCUQY ELECTRODE/ QAPIO POLAROGRAPHY OF URANIUM IN 1 YOLAR HYDROFLUORIC ACID WITH A VERTICAL ORIFICE T 6PA-02-OeR BERYLLIUM FLUORIOF - ZIRCONIUM FLUORIDE ( 65.6-29.4-5.0 MOLE PERCFNT I FVIOENCE FOR ADS'IRPTIPN OF URANIUM 6PPRR-Ci2 YOLECULAR ANATOMY PROGRAM/ 6Qb-04-03 FFECTS OF TEMPERATURES ON THE SPECTRUM CF URANIUM(4+1 IN MOLTEN BERYLLIUM FLUORIDE - LITYIUM FLUORIDt MIXT 68PRR-COb SPECTROPHOTOMETRIC STUDIES OF SOLUTE SPECIES IN MOLTEN FLUORIDE MEDIP/ 48PRR-124 ANALYTICAL METI-OOS FOP THE IN-LIhE ANALYSIS OF MOLTEN FLUCRIOE SALTS/ 68A-C3-C2 IRCN(II1. NICKFL(Illr CkQOMIUM(I1)r AN0 CHROMIUM(II1l IN YOLTEN FLUORIDE SALTS I/ ABSORPTION SPECTRA OF SE 68A-03-CZG ON0 WINDOWED CELL FOR SPECTROPPOTO4ETRIC YEASUREMENTS OF MOLTEN FLUORIDE SALTS I/ CCIUTAINERS FCR MOLTEN FL tF!A-03-02F ASUREMENTS IN MOLTEN FLUORIDES ( REFERENCE ELECTRODE FOR MOLTEN ELUORIOE SALTS I/ ELECTROMOTIVE FORCE ( EM 6PA-03-02C MEASUREMFNTS OF YOLTEN FLUORIDE SALTS I/ CONTAINERS FOR MOLTEN FLUORIDE SALTS ( DIAMOND WIN@OW€D CELL FOR 68A-03-O2F ECTRDCHFMICAL mc SPECTROPHOTOMETRIC STUDY OF SOLUTES IN MOLTEN FLUORIUE SALTS ( ECECTROCHFPISTRY OF TANTA 6 8A- 03- 02 I ABS@RPTION SPECTRA OF SEVERAL TRANSITION METAL IONS Ih MOLTEN FLUCRIDE SOLUTION/ 6PPRR-123 BSORPTION SPECTRA OF SEVERAL 30 TR4NSITION METAL IONS IN MOLTEN FLUORIDE SGLUTICN ( ABSORPTION SPFCTRA OF t8A-03-02G IDE SALTS )I ELECTROMOTIVE FORCE ( EMF I MEASUREMENTS IN MOLTEN FLUORIDES ( REFEREYCE ELECTROOF FOP MrJLTEN 4RA-03-02C IUM FLUORIDE - LITHIUM FLUORIDE MIXTURES/ CONTAINMENT OF MOLTEN FLUORiOES IN SILICA I. EFFECTS DF TEMPERA 68PRR-CO6 FLUORO BERYLLATE I OISPROPORTIONATION OF URANIUMIIVI IY MOLTEN LITHIUM FLUORIDE - BERYLLIUM FLUCRIPE I/ S 58A-03-02E ORTIONATION OF FLECTPOCHEMICALLY GENERATFO URANIUM(V1 IN MOLTEN LITHIUM FLUORIDE - SERYLLIU" FLUORIDE - ZI 6 RA-03-02 A RCONIUM FLUORIOF PT 5OK/ VOLTAMMFTRV OF CHROMIUM(I1) IN MOLTEN LITHIUM FLUORIDE - RERYLLIUY FLUCIRIOE - 21 6eA-03-028 URANIUM( IVll ELFCTROCHErMICAL REDUCTION OF URANI UMI I VI IN MOLTEN LITHIUM FLUGRIOE - EERYLLIUM FLUORIDE - ZI 6PPRR-072 ORTIONATION OF ELECTROCHEMICALLY GENERATE0 URANIUM(V1 IN MOLTEN LITHIUM FLUORIOE - eERYLLIUM FLUORIDE - 21 68PRR-C23 ORT TRPNSITION TIMES/ ELECTROREOUCTION OF URANIUM(IV1 IN MOLTEN LITHIUM FLUORIDE - BERVLLIUM FLUPRICIE - 21 6BPRQ-lOe ORTIONATION OF ELECTR3ChEMICALLY GENERATED URANIUMfVI IN MOLTEN LITHIUM FLUORIOE - BERYLLIUM rLUCRIOE - ZI CRPRP-109 LUORIOE AT 500CI VOLTAMMETRIC STUDIES OF CHROMIUM(I1I IN MOLTEN LITHIUM FLUORIGE - PERYLLIUM FLUORIDE - ZI 68PRR-110 POLTEN FLUORIDE SALTS ( ELECTROCHEMISTRY OF TPNTALUM IN (VOLTEN LITHI(Jfl FLUORIDE - SODIUM FLUOHIDE - POTAS 68A-03-021 TION AN0 SPECTROPHOTOMETRIC MEASUREYENT OF COPPERlIIl IN MOLTEN LITHIUM FLUORIDE - SODIUM FLUORIDE - PflTAS 68A-03-021 IOE I/ SPECTRAL STUDIES OF URANIUM(V1 AN0 URANIUMlVIl IN MOLTEN LITHIUM TETRA FLUORO BEQYLLATE ( GISPfiflPCIF' 68A-03-O2E MOLTEN SALT REACTOR EXPERIYENTl 6RA-03-01 HOO FOR THE OETERMINATION OF URANIUM(III1 IN RADIOACTIVE VOLTEN SALT REACTOR FUEL/ A TRANSPIRATION YET 68PRR-087 PROTON REACTION DETERMINATION OF LITHIUM AN0 FLUORINE IN MOLTEN SALT REACTOR GRBPHITE/ 68A-06-048 OETERMINATION OF FLUORIDE IN A MIXTURE OF MOLYBDENUM FLUOR1DES/ h8B-10-06 MPARISON OF MEASUREMENTS OF THE RADIONUCLIDES -57, MOLYBDENUM-99 - TECHNETIUM-99M. AN0 TECHhETIUM-"9 68A-C 8-C? A BERY LL AT E / SPECTRUM OF MOLYBOENUM(1 I1 I FLUCRIOE IN LITHIUM TETRA FLIJCYO 68A-03-02H DESIGN AND EVALUPTION OF A DELAYED NEUTRON LEACHED HULL MONITOR/ THE 68PRR-059 A FILY RECORDING RADIATION EVENT MONITOR FOR PULSE0 X AN0 GAYMA RADIATION/ 68PRP-011 RGE GAS CROY IN REACTOR TESTS OF REACTOR FUEL FLEMENTS ( MONOPOLE 600 RESIDUAL GAS ANALYZER I/ ANALYSIS OF 68A-O3-C3A EPT.. 196B/ ANALYTICAL CHEMISTRY RESEARCH AN0 OEVELOPMFNT MONTHLY SUMMARY - NOV.71967 / OEC.91967 / JAN.vl9 68PRR-060 AMINO ACID SEQUENCE OF MOUSE HEMCGLOBlNl 68A-04-03H METRY OF FISSION PROCUCTS DEPOSITED IN COMPONENTS OF THE MSREl MEASUREMENT eY GERMANIUM - LITHIUM GAMMA SP 68A-OR-fl4C... IN REACTOR PENETRATION OF FISSION PRODUCTS INTO MSRE PNO PYROLYTIC GRAPHITE/ 68A-08-04D PRECISE DETERMINATION OF URANIUM IN MSRE FUEL/ eee- IC-14 IN GASES I/ DETERMINATION OF URANIUM(II1I IN RADIOACTIVE MSRE FUEL BY HYDROGEN RECUCTION ( ABSOKPTION - TH 688-03-018 FLUORIDE IN MSRE FUEL, PYRnLYLIS METHOD/ b8PRR-081 ANALYSIS OF MSRE HELIUM FGR HYOROCARBONS/ 681-03-010 DETERMINATION OF TOTAL REDUCING POWER OF RADIOACTIVE MSRE SALTS/ 68A-03-GlC - URPNIUM(IV1-233 FLUORIDE I/ DETEPMINATION OF OXIDE IN MSRE SALTS BY HYOROFLUORINATION ( DETERMINATION 0 68A-03-01 A THF ROLE OF THE LAQGE NATIONAL RESEARCH LABORATORIES IN THE USA/ 68PRR-100 GRbPHITE ELECTRODE I/ VOLTAMMETRIC STUDIES OF PLUTONIUM, NEPTUNIUM, AN0 AYERICIUM ( ROTATING PLATINUM DISK 68A-02-070 REPORT OF FOREIGN TRAVEL TO FRANCE, ITALY, GERMANY, THE NETHERLANOSi AN0 HARWELLt ENGLAYDI SEPT-5-2671967 6ePRR-058 TRAVEL TO ENGLAND, SWITZERLPNOv ITALY, GERMANY, AN0 THE NETHERLANDSI JULY-10-31~1968/ REPORT OF FOREIGN 6@PRR-C71 ON GENERATOR STUDIES ( DETERMINATION OF OXYGEN BY 14-MEV NEUTRON ACTIVATION I/ 14-MFV NEUTR 68A-08-05A DETERMINATION OF FLUCRINE IN FLUORSPA? 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FLUORIDE I/ OETERMIhATlON OF DXIDE IN MSRE SALTS BY HYOROFLUURINATION ( OFTFRM h8A-03-01A ON OF HAFNIUM AND ZIRCONIUM IN HAFYIUM OXIDE - ZIRCONIUM OXIDE MIXTURES/ OETFPMINATI 68R-10-07 / CHROMATOGRAPHY / DISSGLUTICh / FUSION / ION EXCHANGF / OXYGEN - TO - METAL QAT10 / PLUTONIA / PROTACTINI 688-1 2-01 BULK DENSITY / CYANIDE / FLUORIDE / POTPSSIIJM CHLORIDE I OXYGEN / PYCNOMETER / SEbLEO TU9E OISSOLUTIOV / T 685-12-02 Ai€R / CPPBON C1 OXIDE )I OEAERITION SYSTEMS I DISSOLVED OXYGEN / SALINE WATFP / INTEPFERENCES TO WINKLER ORA-02-04C 14-MEV NEUTRON GENERATOR STUDIES I OETERMINPTION OF OXYGEN BY 14-MEV NEUTRON ACTIVATION I/ 6PA-08-05A SURFACE IONIZATION OF URPNIUM(IV) FLUORIDE AT VARIOUS OXYGEN PRESSUPESl ~~A-M-o~A NFORMPTION EXTENSION/ INFOPMAT1 ON P4CKAGES SUBMITTED TG THE DIVISION OF TECHNICAL I 684-01-22 DECAY OF PALLAOIUM-103 - RHCDIUM-I03H/ 68P-08-03E PY ( TRbNSFER RIP0 NUCLEIC 4CIOS / TRPNSFER RNA I FILTER PAPER DISK TECHNIQUE )/ INSTRUMENTATION FOQ ANdLY tPA-01-15 NSFER RIBG NUCLEIC ACID/ A SEMIAUTOMATEO FILTER PAPER DISK TECHNIQIJE FJQ THF OETEQMIN&TION OF TR4 6ePRR-003 17 DIONE / DI BROMO FLUORENE / TQUXENE / UREA / VARCUM / PAP1 I FURFURAL / HIPPURIC ACID / CARYCPFYLLENC / 688-11-04 YL SULFOXIDE I HEX4 YETHYL PHOSPHORIC TRI AMIDE / BARIUM PARA ETHYL BENZENE SULFONATE / ESTPOLULACTONE / 2 688-11-04 ASSIUM HEX4 CYANO DI NICKELATE(I1 / POTPSSIUM NICKELIIV) PARA PER IOOPTE !/2 WATER / POTASSIIIM TETQA CYANO 6RA-09 TRY/ A STUDY OF PARPMETERS THAT AFFECT AUALYTICAL ALPHA SPFCTROME 68A-08-02E ORAU RESEARCH PARTICIPANTS/ O~D-I~-OZ 0 2000 MICRONS RY SEOIMFVTATION ANALYSIS/ PARTICLE SIZE OISTRIRVT17N ilF PARTICLES FROM 19 T 68PRR-007 N ANALYSIS/ PARTICLE SIZE OISTRIRUTION OF P4RTICLES FROM 10 TO 2000 YICRONS BY SE3IMENTATIO 68PRR-nO7 lUM/ INTERACTIONS OF HELIUY-3 PARTICLES WITH BORON, NITROGENl SCIOIUM AN0 SERVLL 68PRR-015 OLYTIC GRQPP'ITEI IN REACTOR PENETRATION OF FISSION PRODUCTS INTO MSRE ANI) PYR 6 eA-08-04D ON EXCH4NGE RESIN )I COLUMN CHROMATOGRAPHY WITH ANTIMONY PENTA OXICE ( SEPARPTIOY OF S@DIUM I CHELEX-100 C 6"A-02-05A TED STPTE OF URANYL ION/ ABSORPTION OF THE URANYL ION IN PER CHLORATE MEDIA Ill. RESOL'JTICN OF THE ULTRAV 69PRR-DC8 RADIOLYSIS OF PER CHLORIC AGIO/ 6EA-OB-07C DETERMINATION OF PER FLUORO METHYL cycLa HFXANE IN METHANE/ 654-02-01F M HEXA CYANO DI NICKELITE(1) / POTASSIUM NICKEL(IV1 PARA PER IODATE 112 WATER / POTASSIUM TETQA CYANO NICK 6RA-09 HYCROGEN / NITROGEN I/ uO0lFICATION AN0 INSTALLATION OF PERKIN - ELMER MODEL-240 ELEMENTAL ANALYZER IN A 6 8 A-02- 37E QUE/ GEL PEPYEATION CHROMATOGRAPHY AS A SEPARATIONS TECHNI SRR-lC-?lC GRAPHY OF POLY NUCLEAR AROMATIC HYOROCAQBONS~ALKALGIOSt PHENOLS, AN0 ACIGS I/ EXPLORATCRY STUCIES ( GAS C 6@A-O2-C3A 4GNETIC RESONANCE SPECTROMETRY ( CINNAMYLIOENINOENE / DI PHENYL BFNZO FULVFNE / POLY YFTHYLENE POLY PHENYL 688-11-04 ENINOENE / 01 PHENYL PENZO FULVENE / POLY METHYLENE POLY PHENYL IS0 CYANPTE / FURFURYL ALCOHOL / FURAN ALO 68B-11-04 ER / POTASSIUM TFTRA CYAYO NICKELATE(I1) / TETRA KIS TRI PHENYL PHCSPHITE NICKEL(0) I/ INORGANIC PREPARATI 686-09 OMEDICbL APPLICATI7NS ( FREE FATTY ACIDS / AYINO ACIDS / PHENYL THIO HYDANTOIN DERIVATIVES OF AMINO ACIDS 6@P-C2-010 HYOANTDIN OERIVLTIVES OF AMINO ACIDS / TRI METHYL SILYL PHENYL THIO HYDANTOIN DERIVATIVES OF AMINO ACIDS 48A-02-01C FLUORCMETRIC OETERMINPTION OF PHOSPHATE/ 68A-02-04C PHOSPHATE / 01 METHYL BUTYL PHOSPHATE / METHYL 01 BUTYL PHOSPHATE )/ DETERMlhATION 3F THE METHYL ESTERS 0 688-02-01E THE METHYL ESTERS OF BUTYL PVOSPHORIC ACIDS ( TRI YFTHYL PHOSPHATE I 01 METHYL BUTYL PHOSPHATE / METHYL 01 68A-02-01F HOSPHORIC ACIDS ( TRI METFYL PHOSPHATE IO1 METHYL BUTYL PHOSPHATE I YETHYL CI BUTYL PHOSPHATE )I DETERMIN 68A-02-01E ONIC BEDS / ALGAL NUTRIENTS I/ EUTROPHIC W4TER SYSTEMS ( PHOSPHATE / NITRATE / TECHNICOY AUTOANALYZER / HY 5RA-02-046 RFMCVAL OF PHOSPHPTE ( ELECTRCDIALYSIS )/ 68A-fl5-C7B TASSIUM TETRA CYPNO NICKELATE(I1) I TETRA KIS TRI PHENYL PHOSPHITE NICKEL(G1 I/ INORGANIC PRFPARATIONS ( b 684-09 OIUM / BODY FLUIDS ANALYSES I FLUORESCENCF OF STEROIDS / PHOSPHORESCENCE OF STEROIDS )/ STEROIDS ( GELMAN 58A-02-321: LENE ( TEFLON I AS AN ADSORBENT ( 01 2 ETHYL HEXYL CRTHO PHOSPHORIC ACID / HDEHP / LIQUID ION EXCHANGERS ) 4RA-02-01B LbIMlNG 4MINO ACIDS - CARBON-14 I DI 2 ETHYL HEXYL ORTHO PHOSPHORIC ACID / HDEHP / LIQUID ION EXCHAtVGCRS ) 68A-04-ClG PHGSPHbTE I/ DETERMINATION @F THE METHYL ESTERS OF BUTYL PHOSPHORIC ACIDS ( TRI METHYL PHOSPHATE / 01 METY 6BA-OZ-OlE UPYL PLCOHOL / OEUTERO 01 METHYL SULFOXIDE / HEXA METHYL PHOSPHORIC TRI AMIDE / BARIUM PARA ETHYL BENZENE 688-1 1-04 ALPHA RADIATION 04MAGE IN INORGANIC PHOSPHORS/ CRA-Oe-OZC IS0 CYANATE / FURFURYL ALCOHOL / FJRAN ALOEHYOE / ORGAN0 PHOSPHORUS POLYMEQS / 5 FURFURYL FURFURYL ALCFHCL 68B-11-04 AND MODEL-64-?171/ FILTER PHOTOKETERSI REMOTELY OPERATED, ORNL MODEL-8-1734 tPPRR-073 USE OF STATISTICAL TECHNIQUES IN FLAME PHOTCMETRY/ 684-01-18 IGITAL INSTQUMENT COMPUTER SYSTEM ( POLAROGRAPHY I FLAME PHOTGMETRY / SIGNAL AVERdGING AUTOMATION / CIRCUI 68A -01-21 PTIONS OF THE SECONDPRY EFFECTS OF RdOIATION - PQECISIONI' PHOTOMETRY USING 4 RAOIOISOTOPIC LIGHT SOURCFl AN 6BPRR-031 E OAK RICGE ELECTRON LINEPR ACCELEQATOR ( DRELA I/ PHOTON AND FAST NEUTRON dCTIVATlON ANPLYSIS AT TH 6 @A-08-0 lB ES OF UNEVEN FLUX/ 41R FLOATING SPHERE FOR HOMOGENEOUS PHOTON AND NEUTRON IRRADIATION IY P.EMOTE FACILlTl 68A-08-01A RGYl PHOTOVOLTAIC CONVERSION OF RAOIOISOTOPE DECAY ENE 68A-08-028 PHYSICAL TECHNIQUES OF ACTIVATION/ 6RPRR-C04 NEW ORNL MODEL-Q-1348C PIPETTERl 68A-01-03868PRR-OS4 SERVO CONTROLLED PIPETTERSl PLANNED USE WITH SPECIAL INTERFPCES/ 688-01-216 TUOIES OF PLUTONIUM, NEPTUNIUM, AN0 AMERICIUM l ROTATING PLATINUM DISK ELECTSOOE I ROTATING PYROLYTIC GRAP 6BA-02-070 FLUORIDE MELTS ON VOLTAYMETRY AT PYROLYTIC GRAPHITE AND PLATINUM METAL ELECTRODES )I SIMULTANEOUS ELECTPO 688-03-021 ON / FUSION / ION EXCHANGE / OXYGEN - TO - METAL RATIO / PLUTON14 / PROTACTINIUM / TRANSURANIUM ELEMENTS / 688-12-01 MICRO TITRATION OF PLUTONIUM/ 69A-02-07C SPECTROPHOTOMETRIC._ DETERMINATION OF PLUTONIUM/ 6BA-02-071 BOOK REVIEW OF, ANALYTICAL CHEMISTRY OF PLUTONIUM/ 6BPRR-035 PLUTON1UMlVI)I SPECTRDPCOTOMETRIC DETERMINATION OF TOTAL PLUTONIUM - CBSERVATIONS ON THE REACTIONS BETWEEN 6BPRR-C38 E ( 4PDC I )I DETERYINATION OF CADMIUM IN PLUTONIUY ( AMMONIUM PYRROLIOINE 01 THIO CARBAMAT 684- 05-04B PYROLYTIC GRAPHITE ELECTRODE I/ VOLTAMMETRIC STUDIES OF PLUTONIUM, NEPTUNIUM, AN0 AMERICIUM ( ROTATING PL 68A-02-070 IUM - OBSERVdTIONS ON THE REACTIONS BETWEEN ARSENAZO AN0 PLUTONIUM(1II)r PLUTONIUM(1V) AN0 PLUTONIUMlVll/ h8PRR-038 NS ON THE REACTIONS BETWEEN ARSFNAZO AND PLUTONIUM(1IIIr PLUTONIUM(1VI AND PLUTONIUM(VI1I SPECTROPHOTOMETR 68PRR-038 S BETWEEN 4RSEN4ZO AN0 PLUTONIUM(III)* PLUTONIUM(1V) AVO PLUTONIUM(VI)/ SPECTPOPHOTOMETRIC DETERMINATION 0 hRPRR-03R C POLdROGRAPHYl A CONTROLLED POTENTIbL AND OERIVATIVE DC POLAROGRPPH - ADVANTAGES OF GAP,ID AN0 OERIVATIVE 6eA-01-06 ME CONTROLLER/ ORNL MODFL-8-2792 CONTROLLED POTENTIAL OC POLAROGRARH AND ORNL MODEL-Q-2942 POLAROGRAPYIC D 6 BA- 0 1- C9 CONTROLLED POTENTIAL GC POLAROGRPPH VOLTAMMETER / YODEL-Q-27921 68PRR-C50 AL ORIFICE RAPID TEFLON D.M.E. FOR OBTAINING FUNDAMENTAL POLAPOGRAPHIC DATA/ EVALUATION OF VERTIC 68A-02-ORA 135

RAP10 SCIN POLbROGR4PHIC DETERMINATION OF URANIUM/ 68P-10-09 CNTROLLEO DOTFNTIAI CC PqLPRGGRAPH AN0 CRNL YOOEL-0-1942 POL4ROGRPPHlC DROP TIME CONTROLLER/ ORNL MOOEL-Q- 68A-01-0s / POLAPOGR4PHIC OROP TIME CONTROLLER I MODEL-Q-2942 68PRR-049 RCURY ELECTRODF ( 3.M.E. )I POL4ROGQAFHIC STUCIES WITH THE TEFLON DROPPING ME 68A-02-C8 AL OC POLAROGRAPHY / BODY FLUIDS AN4LYSES PROGRIM J/ PCL4ROGRAPHIC SUQVEY OF BIOCHENICALS ( DIFFE9ENTI 684-01-08 ELECTRICAL 4NC ELECTQOCbEMICAL TESTS @F PERFORKANCE OF POLPROGRIPHSI 684-01-05 GN OF TlMF AVEQAGING AN0 TIME OERIVPTIVE CI9CUITS COR 3C POLPROGR4PHSl OC51.~. 68A-01-1C USE FOR OIGITIL POLAROGR4PHY/ 68A-01-21D

PECE,'.IT POV4NCES IN DIFFERENTIAL POLAROGRLPHYl~~ 68PRR-119 L DESIGN FOR MINIMIZING IR ERROR IN CONTROLLED POTENTIAL POLPROGRAPHYl 4 GEL 68PRR-083 D PDTFNTl4L OIFFERFNTIAL OC PCLAROGRPPNY V. SUSTPACTIVE POLAPOGRPPHY/ CONTROLLE 68PRR-033 E OC PCLPROGRAPH - 4CVAYTAGFS OF RAP10 AYD DERIVATIVE OC POLdROGR4PHYl 4 CCNTPOLLED POTFNTIAL 4Y0 DERIVATI 68A-Ol-CO CGNTROLLED POTSNTIBL DIFFERENTIAL OC POLbROGRAPHY V. SUETRACTIVE POLbROGR4PHYI 68PRR-033 RqPPING MERCURY ELECTROCES ( C.V.E. I I FIRST OERIVATIVF POL4POGRPPHY I/ APPAPATUS FOR PRECISE CONTROL OF 68A-01-04 POLPROGQAPHTC SURVEY OF RIOCVFYIC4LS ( OIlFERENTI4L OC POLIROGRAPHY / BOGY FLUIDS ANALYSES PPOGRAM I/ 684-01-08 L APPLICATIONS OF A DIGITAL INSTRUMENT COMPUTER SYSTEM ( tUL4ROGRAPHY / FLAME PHOTOMETRY / SIGNAL AVERAGIY 68A-01-21 UEOUS HYDQ@FLUCRIC ACICl FOLAROGR4PHY OF SULFUR DI CXIOE I SULFITE ) IN 4Q 68A-02-08C ERTICAL GRIFICE TEFLCN CROPPIKG MEQCURY ELECTROOE/ RLDIO PDLAROGRdPHY CF URANIUM IN 1 MOLAR HYDROFLUORIC 4 684-02-088 METHYL SULFOXIOEl POL4ROGRAPHY OF ZIRCONIUM IY ACETONITRILE AN0 01 6EA-01-07 PECTQUM GF POLY TETRA CLUOQC ETHYLENE I MASS SPECTRUY 01 POLY ETHYLENE IlNE - CELLULOSE / MASS SPECTRUY 0 684-02-O2F )I CONSTITUSNTS 0' TR4NSFER RIP9 NUCLEIC ACID I TRN4 ) I POLY ETHYLENE IUlNE - CELLULOSE / NUCLECSIDES / N 69A-02-02C LEOTIDES 9Y TWIl DIMENSICNAL THIN LAYER CHROMPTOGPAPHY ON POLY ETHYLENE IMINE CELLULOSE/ RESOLUTION OF COKP 68PRR-027 PCMETRY I CINN4YYLICLNINnENE / 91 OHENYL SEN20 FULVENF I POLY METHYLENE P@LY PHENYL IS2 CYANATE / FURFURYL 688-11-04 ANC ACIDS )I FXPL@QbTCQY STUCIES I G4S CHROlATOGQPPHY OF POLY NUCLEAP AROMATIC HY@ROCARBONS1 ALKALOIDS, PH 58A-O2-C3A MYLIDEYIYOEYE / DI OHEFlYL SENZC IULVENF / PJLY METHYLENE POLY PHENYL ISC CYbNATE / FURFUQYL ALCOHOL / FUQ4 68B-ll-C4 ISOLATED BY THIY LAYER ChROY4TOSRAPHY ( M4SS SPFCT9lJ.I OF POLY TETR4 FLliORO ETHYLENE / MASS SPECTRUM OF POL 68A-02-02F ORTHO PFOSPHORIC BCIO / HOEbP / LIQUID ION EXCHAYGERS J/ POLY TETRA FLUOR0 ETHYLENE I TEFLON 1 AS AN ADSOR 688-02-028 / FURFURYL PLCOHOL / FUQbN ALOEHYOC / ORGAN0 PHOSPHORUS POLYMERS / 5 FURFURYL FURFURYL ALCOHOL / DEUTERO 680-11-04 PECTRU,4 OF MERCK SILICA GEL G I MASS SPECTRUM OF CORYING POPOUS GLPSS 7035 / MbSS SPECTRUM OF GELYPN ITLC- 688-02-02F RORATORY I BISMUT? / BULK DENSITY I CYPNIOE / FLUOPIOE I POTASSIUM CHLCRIDE / OXYGEN / PYCNOMETER / SEALED 688-12-02 OPPERIIIJ IN MOLTEN LITHIUM FLUORIDE - SODIUM FLUORIDE - POTPSSIUM FLUORIDE / EFFECT OF OXIDE AN0 HYOROXIO 68A-03-021 TANTALUM IN MOLTEN LITHIUM FLUORIDE - SODIUM FLUOQIDF - POTASSIUM FLUORICE / ELECTROCHFMICAL C-ENERATI@N 4 684-03-021 OROXIOE IYPURITIES IN LITHIUM FLUORIDE - SODIUM FLUCRIOE POTASSIUM FLUORIDE MELTS ON VOLTAMMETRY AT PYROLY 6RA-03-021 I NICKFL-64 - ALUNINUM BLIOY I NICKEL-61 - IRON ALLOY I POTISSIUM HEX4 CYAUO 01 NICCEL4TE(IJ I POTASSIIJM 684-00 tl - lRnN ALLOY / PQT4SSIUM HEX1 CY4NO 01 NICKELATEIIJ / POTASSIUM NICKELIIV) PIRA PER IODATE 112 WbTER / 686-09 TE(IJ / "IT4SSIUi.I NICKELIIVJ PAR4 PER IOOATE 1/2 WATEQ I POT4SSIUM TETRA CYANC NICKELATE(I1) / TETRA KIS T 68A-09

EQ/ CONTROLLED POTENTI4L AN0 CONTPOLLEO CURRENT CYCLIC~~ VOLTAMMET ~~ 68PRR-051 ES OF RAPID AN0 DERIVATIVE OC POLPROGRAPHYI A CCNTROLLFD DOTENTI4L AN0 DERIVATIVE DC POLAROGRAPH - 40VdNTA 684-01-06 CONTROLLFO POTENTIAL CONTR7LLCC CURRENT CYCLIC VOLTAMNETERI 6SA-01-12 DERIVATIVE CIRCUITS F3R USE WITH THE CONTROLLED P3TENTIAL CONTROLLEC CURRENT CYCLIC VOLT4MPETERI 48A-01-13 4!4ERICIUM-241 / HALF LIFE OF AMERICIUM-243 I/ CONTROLLED POTENTIAL COULOMETRIC OETEKMINATION OF 4MERICIUM 684-02-074 SOLI3 STATE CONTROLLED POTENTIAL COULOMETRIC TITR4TORI 6e~-oi-oi 4 I/ MOOIFICATIONS TO THE HISH SENSITIVITY CONTROLLED POTENTIAL COULOMETRIC TITRATOR ( ORNL MODEL-0-256 68A-01-02 APHIC OROP TIME C@YTRCILER/ OANL MODEL-Q-2792 CONTROLLED POTENTIAL OC POLAROGRAPH AN0 ORNL MODEL-0-2942 PO 684-01-09 92/ CONTROLLED DOTENTIAL OC POLAQCGRADH VOLTAMMETER / MODEL-(3-27 68PRR-050 CTIVE PCLAROGRAPHYI COYTROLLEO POTENTIAL DIFFERENTIAL CC POLAROGRAPHY V. SUflTRA 68PQR-C33 IONIZATION POTENTIAL MEPSUQEMENTS/ 684-06-030 4 CELL DESIGN FOR MINIMIZING IR ERRSR IN CONTROLLED POTENTIAL POLAROGRAPHY/ 68PRR-083 CYCLIC VOLTAAMETERI CONTROLLED POTENTI~LI CONTR9LLEO CURRENT/ 68PRR-072 COULL?MMETRIC TITRATOZv CONTROLLcO POTENTIAL, HIGH SENSITIVITYt ORNL MODEL-Q-2564/ 68PRR-077 SUQFACE IONIZATIDU 111. THE FIRST IONIZATIOY POTENTIALS OF THE LINTHPNIOFSI 68PRR-016 QY ELECTRODE VCLTAMMETRYl ON THE SEPARATION Or HALF-WAVE POTFNTIALS RFQUIREC FOR RESOLUTI@N OF SIMPLE, REV 684-01-14 RY CLECTR?OE VCLTbMMCTRY/ ON THE SEPhR4TION OF HPLF-WPVE POTENTIALS RE2LlIRED FOP HESOLUTIOY OF SIYPLE. QFV 68PPR-025 AUTOMATIC POTENTIOMETRIC TITRATOR/ 68PRR-052 EL-Q-1728 AN0 MODEL-Q-17284l AUTOMATIC POTENTIOMETRIC TITPATCUT VELOCITY SERVO, ORNL MOD 68PPR-078 TREF'O IF' 4TOMIC POWER GENERATION AND URANIUY RESOURCES/ 68TR-02 DETERYINATION OF TOTAL REDUCING POWER OF RADIOACTIVE MSRE SALTS/ 68A-03-01C THEORY AN0 PRACTICE OF LIQIJID SCINTILLATIqN COUNTTNGl 68PRR-117 RDCHLORIC ACID/ HOMOGENEOUS PQECIPITATIONS USING R4DIOLYTICALLY GENERATED YYO 68PRR-103 .M.E. ( LIPST OERIVPTIVE POLhPOGR4PHY )I 4PPARATUS FOR PRECISE CCNTROL OF MEQCURV FLOd R4TE OF DROPPING 68A-01-04 PRECISE DETERMINATION OF URANIUM IN MSRE FUEL/ 680-10-14. PRECISE DETERMINATION OF UR4NIUM-235/ 684-08-04A CAL APPLICATIONS OF THE SECONEbQY EFFECTS OF RAOlATI3N - PRECISION PHOTOMETRY USING 4 PLDIOISOTOPIC LIGHT 68PRR--031 MISCELLANEOUS TRACE OFTERMINATIONS INVOLVING CHEMICAL PRECONCENTQATIONI 6a~-05-04 CHEMICAL PRECONCENTRATION OF TRACE ELEMENTS IN BONE ASH/ 684-05-03 VALIOITY OF SOME TESTS CF INTELLECTUAL AalLITY KO2 PREOICTING GRADES IN RELATED CRAFT TRAINING/ 6RPRR-005 I TETRA KIS TRI PHENYL PHOSPHITE NICKELIOJ )I INORGINIC PREPARATIONS ( AMMONIUM AZIDE / CALCIUM - GOLD AL 6RA-09 PREPARITIVE GAS CHRDMATOGRPPHY ( VARIAN-AFROGRAPH PREPARATIVE GAS CHROMPTOGRPPH I/ 68A-02-01G PREPARATIVE GAS CHRCMATOGRAPH I/ PREPARATIVE GAS CHRGMATOGRAPHY ( VARIAN-AEROGRAPH 68A-02-01G STRESS PNALYSIS IN TAPERED TRANSITION JOINTS IN REACTOR PRESSURE VESSEL/ 68TR-01 4CE IDNIZATION OF URANIUM(IV) FLUORIDE AT VIRIOUS 3XYGEN PRESSURES/ SURF 684-06-03A PQEVIOUS STATUS OF PROBLEM/ 688-05-058 STRONTIUM-92, PRODUCT AkALYSIS GUIDE/ 68PRR-074 STPONTI UM-90, PRODUCT ANALYSIS GUIOEI 69PRR-075 FISSION PRODUCT RELEASE FR'IM REACTOR FUEL MICROSPHERFSI 68A-08-04F EXTRALAEORATORY PROFESSIONAL ACTIVITIES/ 68E PPPLICATIONS TO REACTOR PROGRAMS / 688-08-04 GRAOUATE THESIS RESEARCH PROGRAMS/ 680-14-03 SUMMER STUDENT PROGRAMS / 680-14-C5 4NALY TICAL CHEMISTRY DIVISI ON ANNUAL PROGRESS REPORT FOR PERIOD ENDING OCT.31.1967/ 68PRR-055 TIVE INDEXES TO THE PNALYTICPL CHEMISTRY DIVISION ANNUAL PROGRESS REPORTS 1°64-1967/ CUMULA 68PRR-056 STUDIES RELATED TO PROJECT SALT VAULT/ 68A-08-076 COOPEQATIVE PR 0 J EC TS / 684-01-23 PNALYTICPL CHEMISTRY FOR REACTOR PROJECTS/ 6PA-03 PROPORTIONAL BET4 COUNTER, W INOOWL ESSl 68PRR-079 OCEAN SEDIMENTS/ PROSPECTS AN0 PROBLEMS FOR ACTIVATION ANALYSIS OF 68PRR-104 / ION EXCHANGE / OXYGFN - TO - METAL RATIO / PLUTONIA / PROTACTINIUM / TRANSURANIUM ELEMENTS / URANIA / Z 688-12-01 GEL ELECTROPHORESIS OF PROTE INSI 68A-04-03F IN GRAPHITE, USING a SLIT SCANNING TECHNIQUE/ PROTON REACTION ANALYSIS FOR LITHIUM AN0 FLUORINE 68PRR-046 RINE IN MOLTEN SILT REPCTOR GRPPHITE/ PROTqN REACTION OETERYINATION OF LITHIIJM AN0 FLLS 68A-08-048 A FILM RECORDING RADIATION EVENT MONITOR FOR PULSE0 X AN0 GAMMA RAOIATIONl 6BPRR-011 FNTS ( YCNOPOLE 600 RESIOUPL G4S ANALYZER J/ ANALYSIS OF PURGE GAS FROM IN REACTOR TESTS OF REPCTOR FUFL E 681-03-03A REAGENT PURIFICATION/ 68A-05-03A 136

PURIFICATICN OF AMERICIUM-241 ANC AMERICIUM-243/ 68A-02-C7H ITY / CYANIDE / FLUORI9E / POTASSIUM CHLORIDE I OXYGEN / PYCNOMETER / SEALED TtJBE OISS3LUTION / THOilIUM / 685-12-02 RUTHENIUM RAOIOArTIVITY IN AQUFOUS SOLUTIONSt PYRIDINE EXTRACTION - GAMMA COUNTING METHOD/ 68PRR-080 FLIJORIOE IN MSRE FUFLI PYROLYSIS METHOD/ 6RPRR-OP1 IN REACTOR PENETRATION OF FISSION PROClUCTS INTC MSEE AVO PYROLYTIC GRAPHITE/ ~BA-O~-C~O DIUY FLUORIDE POTASSIUM FLUORIDE MELTS ON VOLTAMMFTRY AT PYROLYTIC GRAPHITE AND PLaTINUM YET4L ELECTROOFS 686-03-021 AMERICIUM ( ROTATING PLATINUM DISK FLECTROOE / ROTATING PYROLYTIC GRAPHITE ELECTRODE I/ VOLTAMMETRIC STLID 634-02-C70 DETERMINATION OF CADMIUM IN PLUTONIUM ( AMMONIIJP PYRROLIOINE DI THIO CAQBAMATE ( APOC I I/ 6FA-05-045 QUALITY CCNTROLl 688-12-CO 4 / THULIUM-16P / THLLIUM-170 I THULIUM-171 / TQITIU'' )/ QUALITY CCNTROL ( RAOIOPHARMACEUTICALS / CARBON-1 ~~A-~IR-o~B SION, JULY-SEPT.91967/ STATISTICAL QUALITY CONTROL REPORT. ANALYTICAL CHFMISTPY OIVI 64L"RR-039 SIGN, OCT.-OEC., 1967/ STAT1 STICAL QUALITY CCNTROL REPORT, AN4LYTICAL CHEMISTRY OIVI 58PRQ-C4C SION, JAN.-YAR..1968/ STATISTICbL QUALITY CCNTROL REPORT, ANALYTICAL CHEMISTRY DIVI 6GPRR-041 SION. APR.-JUNF,1968/ STATISTICAL QUALITY CCNTROL REPORT. AYALYTICAL CHEYISTRY DIVI 6ePRR-C42 AIR QUALITY SURVEY/ 681-02-06 C1 METHYL SULFOXIDE/ QUANTITATIVE ELECTRCOEPOSITION OF ACTINIDES FROM 6eA-08-02D ANALYTICAL APPLICATIONS OF CERENKOV RAD1 AT ION/ 46A-08-024 RECORDING RADIATIDN EVENT MONITOR FOR PULSED X AND GAYYA RAD I AT I ON/ b FILM 68PRP-C11 RCEl ANALYTICAL APPLICATIONS OF THE SECONDARY EFFECTS OF RACIATION - PRECISION PHOTOMETRY USING A RAOIOISO 6RPRR-031 RADIATION AND THERMAL STABILITY OF SPRAYS/ CRPQR-125 RADIATION CONTROL AND SAFETY/ 6PR-12-05 ETURNED LUNAR SAMPLES/ LOW LEVEL RADIATION COUNTING FACILITY KO9 GEOCHEMICAL AND K 68A-C8-@2H AI PHA RADIATION DAMAGE IN INOPGANIC PHOSPHURS/ 68A-08-OZC OIAT ION/ A FILY RECORDING RADIATION EVENT YONITCR FOR PULSED X AN0 GAMMA RA 6RPRR-01 1 URANIUM ELEYENTS / URANIA / ZIQCONIA I/ HIGH LEVGL ALPHA RADIATION LABORATORY ( PLPHA bYOROXY IS0 BUTYRIC 688-12-C1 INSTRUMENTATION FOR THE HIGH RADIATION LEVEL ANALYTICAL LABORATORY ( HRL4L I/ 688-01-03 EFFECTS OF RADIATION CN ANALYTICAL METHODS/ 68A-OP-07 EFFECT OF RADIATION ON COMMON ANALYTICAL REAGENTS/ 69A-Ce-C7F THE EFFECT OF RADIATION ON SOME ANALYTICAL METHODS/ 6RPR.R-126 EFFECT OF GAMMA RADIATION ON SPECTROPHOTOMETRIC METHODS FOR lR3NI 66A-OR-07F RADIOLYSIS OF RADIATION SAFEGUARD SPRAY SOLUTIONS/ 686-08-078 RADIOACTIVE CONT4MINANTSI 68A-05-05E ELECTRON MICRCSCOPY OF RAD I OACT I VE MAT Et7 I ALS I 6811-07-CZ PIRATION METHOD FOQ THF DETERMINATION OF URANIUM(III1 IN RADIOACTIVE MOLTEN SALT REACTOR FUEL/ A TRANS 68PkR-087 EN FLUORIDE IN GASFS I/ DETEQMINATION OF URANIUM(III1 IN RADIOACTIVE MSRE FUEL BY HYDRflGEN REDUCTION ( AES 68A-03-01 B OETEPMINATIOY OF TOTAL REDUCING POWER OF RADIOACTIVE MSRE SALTS/ 6r?A-O?-OIC FACILITY FOR SPECTROPHOTOMETRY OF RADIOACTIVE SAMPLES/ 68A-r)3-0?D CLVENT EXTRACTION ISOLATION OF BERKELIUM-749 FROM HIGHLY RADIOACTIVE SOLUTIONS AND ITS DETERMINATION BY BE 68f-10-02 GLVENT EXTRACTION ISOLATION OF BERKELIUM-249 FROM HIGHLY R4DIOACTIVE SOLUTIGNS AND ITS OETEQMINITIDN BY BE 68PPR-013 ACTION - GAMMA COUNTING METHOD/ RUTHENIUM RADIOACTIVITY IN AQIJEOUS SOLUTIONS, PYRIOIME EXTQ 69PRR-CeO RADIOACTIVITY STBNDARCSl 6e4-08-06C NUCLEAR AN0 RADIOCHEMISTRY/ 688-08 R4OIOISOTOPFS - RADIOCHEMISTRY LABORATORY/ 688- 12-04 PHOTOVOLTAIC CONVERSION OF RADIOISOTOPE DECAY ENERGY/ 68A-OP-025 COOPERATIVE ISOTOPES PROGRBM ( RADIOISOTOPES I/ C ?A-08-06 RADIOISOTOPES - RADIOCHEMISTRY L4BOQATORYf 688-12-C4 OARY EFFECTS OF RAOIATIOY - PRECISION PHOTOMETRY USING A RADIOISOTOPIC LIGHT SOURCE/ ANALYTICAL APPLICATIO 68PR R-03 1 T ON ANALYTICAL PROCEDURES/ CHLORINE PRODUCTION BY GAMMA RADIOLYSIS OF ACID CciLORIOE SnLllTIONS AND ITS EFC 6ePRR-019 RADIOLYSIS OF NITRATE SOLUTIONS/ 696-08-078 RADIOLYSIS OF DER CbLORIC ACID/ 66A-08-97C / RADIOLYSIS OF ilADIATION SAFEGUARD SPRAY SOLUTIONS h 8A-0 P-C7A HOMOGENEOUS PRECIPITATIONS USING RAD1OLYT ICALLY GENEQATEO HYOROCHLOR IC ACID/ 68PRR-103 NUCLEAR PROPERTIES OF RADIONUCLIDES/ 686-08-03 AVPILPBILITY OF STANDARDS FOR COMMON RAD1 ONUCL I DES/ 68PRR-C28 HALF-LIVES OF QAOIONUCLIDES IIIl 6BPRR-OZQ M-99MI INTERLABORATORY COPPARISON OF MEASUREMENTS OF THE RADIONUCLIOES COBALT-57. MOLYBDENUM-99 - TECYNETI 48A-OR-03A T WATER/ RADIONUCLIDES IN HIGH FLUX ISOTOPE REACT09 COOLAN 68A-OB-0hH THULIUM-170 / THULIUM-171 / TRITIU4 I/ QUALITY CONTROL RAOIOPHARMACEUTICALS / CAllBgN-14 / THbLIUM-168 / 68A-OF-068 SOME APPROACHES TO MORE RAPID ANPLYSIS/ 6FPRR-OQl POTENTIAL AND CEPIVATIVE OC PCLAROGRAPH - ADVANTAGES OF RAPID AND DERIVATIVE DC POLAROGRAPHY/ A CONTROLLE 6BA-01-06 MUM BOMBARDING ENERGIES IN HELIUM-3 ACTIVATION ANALYSIS/ RAPID CALCULATION OF SENSITIVITIES, INTERFERENCES 6BPRK-030 TIES OF FLUORICE/ RAPID DISTILLATION SEPARATION OF MICROGRAM QUANTI 68PRR-018 TH A VERTICAL ORIFICE TEFLON DROPPING MERCURY ELECTRODE/ RAPID POLAROGRAPHY OF URANIUM IN 1 MOLAR HYDROFLU 686-02-088 /. RAPID SCAN POLAROGRAPHIC DETERMINATION OF URANIUM 688-10-09 ELEMENTS/ NEW EXTRACTION CHR,OMATOGRAPHIC METHOD FOR THE RAPIO SEPARATION OF AMERICIUM FROM OTHFR TRANSURA 688-1 0-03 BY ANION EXCHANGE/ NEW METHOD FOR THE RAPID SEPARATION OF @FRKELIUY(IV) FROM CEQIUMIIVI 688- 10-01 BY ANION EXCHANGE/ NEW METHOD FOR THE qAPI0 SEPARATION OF E!ERKELIUfl(IVl FROM CERIUH(IV1 6RPRR-024 AROGRAPHIC DATA/ EVALUATION OF VERTICAL ORIFICE RAPID TEFLCN D.M.E. FOR ORTAIUIYG FUNOAMENTAL POL 6PA-02-08A CEDURE I/ DETERMINATION OF TRACES OF RARE EARTH ELEMENTS IN BISMUTH ( CARRIER FREE PRO 684-05-046 OGRAPHY I/ APPARPTUS FOR PRECISE CONTROL OF MERCURY FLOW RATE OF DROPPING YERCURY ELECTRODES ( D.M.E. I ( 688-01-04 E - BERYLLIUM FLUDRIOE - ZIRCONIUM FLUORIDE AT FAST SCAN RATES AN0 SHORT TRANSITION TIMES/ ELECTROREDUCSIfl 6ePRR-108 ISSOLUTION / FUSION / ION EXCHANGE / OXYGEN - TO - METAL RATIO / PLUTONIA / PRnTACTINIUM / TRANSURANIUM EL 688- 12-0 1 PHITE, USING A SLIT SCANNING TECHNIQUE/ PROTON REACTION ANALYSIS FOR LITHIUM AN0 FLUORINE IN GRA 6BPRR-C46 MOLTEN SALT REACTOR GRAPHITE/ PROTON REACTION DETERMINATION OF LITHIUM ANn FLUORINE IN 6 EA-D 8-C4B 14-MEV NEUTRON REACT I ON RES E ARCH/ 6eA-O9-C5D C DETERMINATION OF TOTAL PLUTONIUM - OBSERVATIONS ON THE REACTIONS BETWEEN ARSENAZO AND PLUTONIUM(III1, PL 68PRR-C38 RADIONUCLIDES IN HIGH FLUX ISOTOPE REACTOR COOLANT V(ATER/ 69A-08-06H MOLTEN SALT REACTOR EXPERIMENT/ 68A-03-Cl DETERMINATION OF URANIUM(III1 IN RADIOACTIVE MOLTEN SALT REACTOR FUEL/ A TRANSPIRATION YETHOO FOR THF 68PQR-087 ALYZER I/ 4NALYSIS OF PURGE GAS FRO!4 IN REACTOR TESTS OF REACTOR FUEL ELEMENTS ( MONOPOLE 600 RESIDUAL GAS 6BA-03-038 FISSION PROLlUCT RELEASE FROM REACTOR FUEL MICRDSPHERES/ 68A-OR-04F ION DETERYINATION OF LITHIUM AN0 FLUORINE IN MOLTEN SALT REACTOR GRAPHITE/ PROTON REACT 686-08-045 AND PYROLYTIC GRAPHITE/ IN REACTOR PENETRATION OF FISSION PRODUCTS INTO MSRE 68A-08-040 STRESS ANALYSIS IN TAPERED TRANSITION JOINTS IN REACTOR PRESSURE VESSEL/ 6BTR-C1 APPLICATIONS TO REACTOR PROGRAMS/ 6BA-06-04 ANALYTICAL CHEYISTRY FOR REACTOR PROJECTS/ 68A-03 D RESIDUAL GAS ANALYZER I/ ANALYSIS OF PURGE GAS FROM IN REACTOR TESTS OF 'IEACTOR FUEL ELEMENTS ( MONOPOLE 68A-03-03A ANALYSIS FOR NUCLEAR REACTORS/ 6RPRR-092 REAGENT PURIFICATION/ 68A-05-03A EFFECT OF RADIATION ON COMMON ANALYTICAL REAGENTS/ 6861-08-07E CRTHD PHOSPHORIC ACIC / HDEHP. / LIQUID ION EXCHANGERS I/ RECLAIMING AMINO ACIDS - CARBON-14 ( DI 2 FTHYL H 68A-04-01G ON ANbLYSIS/ THE RECOIL TECHNIQUE AN0 ITS POSSIBLE USE IN ACTIVATI 68PRR-014 D GAMMA RACIPTIONl A FILM RECORDING RADIATION EVENT MONITOR FOR PULSEC X AN 68PRR-011 137

A

R EClVERY OF S ICICON/ 68A-05-05C OETFRMINATIJFJ OF TOTAL REDUCING POWER OF RACIOACTIVE MSRE SALTS/ 6SA-03-01C nASS SPECTXCMETRIC DATA QEOUCTION/ b8A-06-04 ION OF UPANIUM(III1 IN R4CICACTIVF MSRC FUEL BY HYDROGEN REDUCTION ( A8SO?PTlr?N - THERMCL CONDUCTIVITY MEA 684-03-018 EVIDENCE FOR ADSORPTION OF URANIUM(IV1I ELECTROCHEMICAL REDUCTION OF URANIUM(IV1 IY MOLTEN LITHIUM FLUOR1 68PRR-022 CMCTIVE FORCE ( EMF I MEASURECENTS IN MOLTEN FLUORIDES I REFFREhCE ELECTRODE FGR MCLTEN FLUORIDE SALTS I/ 68A-03-02C UPERVISOR - A STATUS RCPORTl STANDARD REFEQENCE MATERIALS AS VIErlEO 5Y THE LABORATCRY S 68PRR-034 OPY IN THE NEUTROhl DEFICIENT MASS NUMBEQ BETWEEN 173-185 REG1 ON/ N UC L F AP SPEC TRC SC 684-08-03D FISSION PRODUCT RELEASE FROM REACTOR FUEL MICROSPHERES/ 68A-08-04F A REMODELED LABORATORY FOR GAS CHROMATOGDAPHYI 684-02-018 SPHEQE FOR HOMCGENFOUS PYOTCN AN0 ;'IEUTPON IRRAOIATION !N REMOTE FACILITIES OF UNEVEN FLUX/ AlQ FL@4TING 686-08-ql A -3171/ FILTFR PHOTOMETERS, REMOTELY OPERATED, ORNL MODEL-8-1734 AN0 MODEL-64 68PRR-073 ATION OF A LIPOPFILIC ACSORPTION RESIN FOR OESALTING AN0 REMOVING OPGANIC CCMPOUNOS FROM WATER ( ACETATE / 68A-0 2-058 ALIEN GUESTS IN RESIDENCY/ 680-14-06 IN REACTOR TESTS OF REbCTOR FUEL ELEMENTS ( MONOPOLE 6DO RESIDUAL GAS ANALYZER I/ ANALYSIS OF PURGE GAS FR 68A-03-C3A XIOF I SEPAQATION OF SODIUM / CHELEX-100 CATION EXCHANGE RESIN I/ COLUMN CHROMATOGRAPHY WITH ANTIMONY PENT 68A-02-05A F LIGANG EXCHANGE CHROMATOGRAPHY ON COPPER LOADED CHELC-X RESIN COLUMNS/ PRINCIPLES 0 68A-04-CZA AMRERLITE XAD-2 I/ EVALUPTIOU OF A LIPOPHILIC ADSORPTION QESIN FOR OESALTING AN0 REMOVING ORGANIC COMPOUND 6861-02-058 / LOh RESOLUTIGN MASS SPECTROMETRY OF OFGANIC COYPOUNDS 688-06-02 N LPYER CHROM4TflGP.PPHY ON POLY ETHYLENE IMINE CELLULCSE/ RESOLUTICN OF COMPLEX MIXTURES OF NUCLEIC ACIO BA 6BPRR-027 I ON THE SEPAPATION OF HALF-WAVE POTFNTIALS REQUIRFD FOQ RESOLUTION OF SIMPLE, REVERSIBLEI OVERLAPPING WAV 68A-01-14 / ON THE SEPARATION OF k4LF-hAVE POTENTIALS REQUIRED FOR RESOLUTION OF SIMPLE, REVERSIBLE. @VEQLAPPING WAV 6ePRR-CZ5 ABSOQPTION OF THE URANYL ION IN PER CHLORATE MEDIA 111. RESOLUTIDN OF THE ULTRAVIOLET BAN0 STRUCTURE - SO 68PRR-008 PPURIC ACID / CARYOPHYLLENE I LIPIDS I/ NLCLE4R MAGNETIC RFSONARCE SPECTPOVETQY ( CINNAMYLIOENINOENE I 01 688-1 1-04 TRE4D IN ATOMIC PEl'AER GENERATION AN0 URANIU!4 RESOURCES/ 68TR-02 EC COMPOUNDS/ CATALOG 06 GAS CHROMATCGRAPHIC RETENTION OATP FOR URINARY CONSTITUENTS AND QELAT 6ePPR-037 OW LEVEL RADIATION COUNTING FACILITY FOR GEOCHEMICAL AN0 RETURNED LUNAR SAMPLES/ L 68A-08-02H HALF-WAVE POTENTIALS REQUIRED FOR RESOLUTION CF SIMPLE, REVERSIBLE, CVEQLAFFING WAVES IN STATIONARY ELECT 684-01-14 HALF-WAVC POTENTIALS qE8UIREO COR RESOLUTION OF SIMPLE? RFVERSIBLE, OVERLAPPING rlAVFS IN STATIONARY ELECT 68PRR-025 BOOK REVIEW OF, ANALYTICAL CHEMISTRY OF PLUTONIUM/ 68PRR-035 3ECAY OF PALL4OIUM-103 - RHO!lIUM-l03MI 68A-08-03E ( DECAY SCHEIIFS / IRCN-55 / BARIUM-140 / SAMARIUM-151 / RHODIUM-103M / RUBIDIUM-84 / IOnlYE-129 / IODINE- 6 EA- 0 e- 060 R PAPER DISK TECHNIQUE F3R THE OETERMINATION OF TRANSFER RIBO NUCLEIC 4CIOI A SEY IAUTOMATEO F ILTF 68PRR-003 DETERMIYATICN OF METHIONINF ACCEPTING TRANSFER RIBO NUCLEIC ACID I METPIONINE TRNA I/ 68A-04-ClB GEL FLECTROPHORESIS OF RIBO NUCLEIC ACID ( RNA I/ 6PA-04-01 J KIYETICS OF AMINO ACYLATICN OF TRAP'SFER RIRC NUCLEIC ACID ( TKNA I/ 684-04-01F OPTIMIZING CONDITIONS FOQ THF DETERi4INATICN OF TQbNSFF8 91913 NUCLEIC CCIO I TRNA I/ A FRACTIONAL FACTORIA 68A-04-01C EOTIOES I NUCLEIC ar.1~QASFS I/ C~NSTITUEYTS 0' TRANSFER RIB0 NUCLEIC ACID ( TRNA 1 I POLY ETHYLENE IMINE 68A-02-OZC OFTFQMINATION OF TYROSINE ACCEPTING TRANSFER RIB0 NUCLEIC ACID ( TYROSINE TRNA I/ 6RA-04-016 HY/ TERMINAL NUCLEOSIDE ASSAY OF RIBJ NUCLEIC ACID BY LIGAND EXCHANGE CHROMATOGRAP 68A-04-011 HYI TERMINAL NUCLEOSIDE ASSAY OF RIBO NUCLEIC ACID BY LIGAND EXCHANGE CHROMATOGRAP 68PRR-009 / INSTRUYENTATIOY FOR ANALYTICAL 8IOCHEMISTRY I TRANSFER RIBC NUCLEIC ACIDS I TRANSFER RNA I FILTEQ PAPER 68A-01-19 AUTOMATED OETERMINATION OF TRANSFER RIB0 NUCLFIC ACIDS I TQNA I/ 6BA-04-010 CHEMICAL ANALYSIS OF TRANSFER RIBO NUCLEIC ACIDS I TRNA I/ 68A-04-01H SCINTILLATION COUNTING DATA IN THE ANALYSIS OF TRANSFER RIB7 NUCLEIC ACIDS ( TRNA I/ CCJMPUTER PROCESSING 6RA-04-01E PHYl ASSAY OF 3/ TERMINAL NUCLEnSIOES OF TRANSCER QIBCI NUCLEIC ACI9S BY LIGAND EXCHANGE CHROMATOGRA 68PPR-085 PHOTON AN0 FAST NEL'TRUN ACTIVATION ANALYSIS AT THE OAK RIOCE ELECTRON LINEAR ACCELERATOR I ORELA I/ 684-08-C1B GEL ELECTROPHORESIS OF RIBO NUCLEIC ACID I RNP I/ 68P-04-01 J PL SIGCYEMISTRY ( TRANSFEQ RIPC NUCLEIC ACIDS / TRANSFER IRNA I FILTER PAPFR DISK TECHNIQUF )/ INSTRUMENTAT 68A-01-19 MMETRIC STUDIES OF PLUTCNllJM, NEPTUNIUM, AN0 AMERICIUM ( IROTATING PLATINUM DISK ELECTRODE / R3TATING PYROL ~~A-OZ-O~D NIUM, AN0 AMERICIUM ( RGTATING PLATINUM DISK ELECTRODE / ROTATING PYQCLYTIC GPAPHITF ELECTPOOE )/ VOLTAMME 68A-02-070 LT NEUTRON IRRADIATIONS/ THREE DIMENSIONALLY ROT4TING SAMPLE HCLCER FOR 14-MILLION €LECTROY VO 68PRR-012 S / IRON-59 / @ARIUM-140 / SAMARIUY-151 I RHODIUM-103M / QUBIOIUM-84 I IODINE-129 / IODINE-130 / YTTRIUM-9 68A-08-060 IOINE EXTRACTION - GANqA COUNTING YETHOD/ RUTHENIUM RAOICJACTIVITY IN AQUEOUS SOLUTIONS, PYR 68PRR-OR0 RADIOLYSIS OF RADIATION SAFEGUARD SPRAY SOLUTICNS/ 68A-08-07A NUCLEAR SAFETY/ 6 8 A- 0 3-03 RAOIATION CONTROL 4N0 SAFETY/ 6 86-1 2-05 R8ON 01 OXIDE )/ DEAERATION SYSTEMS I DISSOLVED OXYGEN I SALINE WATER / INTERFERENCES TO WINKLER METHOD / 688- 02-04C MOLTEN SALT REACTOR EXPERIWFNTI 68A-03-01 THE CETEDMINATION OF URANIUCIIIII IN QA010ACTIVE._ MCLTEN SALT REACTCR FUEL/ A TRANSPIRATION METHOD FOR 6BPRR-087 REACTION DETERMINATION OF LITHIUM 4UO FLUORINE IN MOLTENI SALT REACTGR GRAPHITE/ PROTON 6 8A-08-04B STUDIES RELATED TO PROJECT SALT VAULT/ 68A-08-07G ETERHINATIOY OF TOTAL RFOUCING POWER OF RADIOACTIVE *SRE SALTS/ 0 684-03-01C ICAL METHODS FOR THE IN-LINE AhALYSIS OF MOLTEN FLUORIDE SALTS/ ANALYT 688-03-02 (111, CHROMIUM(IIJ, AN0 CFROMIUM(III1 IN MOLTEN FLUOSIOE SALTS I/ ABSORPTION SPECTRA OF SEVERAL 30 TRANSIT 688-03-02G L FOR SPECTROPHOTOMETRIC MEASUREMENTS OF MOLTEN FLUORIDE SALTS I/ CONTAINERS FOR MOLTEN FLUORIDE SALTS I 0 68A-03- 02 F LTEN FLUORIDES I REFERENCE ELECTRO3F FOR PGLTEN FLUORIDE SALTS I/ ELECTROMOTIVE FORCE I EMF I MEASUREMENTS 68A-03-02C MOLTEN FLUORIDE SILTS I/ CONTAINERS FOR MOLTEN FLUORIDE SALTS 4 DIAMOND WINCOWED CELL FOR SPECTROPHOTOMET 68A-03-OZF 0 SPECTROPHOTOMETRIC STUDY OF SOLUTES IN MOLTEN FLUORIDE SILTS I ELECTROCHEMISTRY OF TANTALUM IN MOLTEN LI 68A-03-021 ANIUMIIVI-233 FLUORIOE I/ OETERMIN4TION OF OXIDE IN MSRE SALTS BY HYDROFLUORINATION ( DETERMINATION OF nxi 68A-03-016 NIOBIUM IN MIXTURES OF FLUORIDE SALTS, SPECTROPHOTCMETRIC THIO CYANATE METHOD/ 6RPRR-082 OTOPE MATERIALS ( DECAY SCHEMES / IRON-59 / BARIUM-140 / SAMARIUM-151 / RHOOIUM-103M / RUBIDIUM-84 / IODIN 68A-08-060 N IRRAOIATIONS/ THREE 0 I YENSIONALLY ROTATING SAMPLE HCLDER FOR 14-MILLION ELECTRON VOLT NEUTRO 6PPRR-012 UTPUT OF A CCNTINUOUS FLOh ANbLYZERI AN AUTOPATIC SAMPLER FOR OBTAINING DISCRETE SAMPLES FROM THE 0 68PRR-021 FACILITY FOR SPECTROPHOTOMETRY OF RADIOACTIVE SAMPLES/ 68~-03-020 ION COUNTING FACILITY FOR GECCHEYICAL AND RETURNED LUNIR SAMPLES/ LOW LEVEL RAOIAT 68A-08-02H YZERl AN AUTOMATIC SAMPLER FOR OBTAINING DISCRETE SAMPLES FPOM THE OUTPUT OF A CONTINUOUS FLOh ANAL 68PRR-021 DEVICE FOR SlMPLING GASES CONTAINEC IN SEALED YETAL TUBES/ 68A-02-C1C RAPID SCIN POLAROGRAPHIC DETERMINATION OF URANIUM/ 688-10-09 UORIOE - BERYLLIUM FLUORIDE - ZIQCONIUM FLUORIDE AT FAST SCAN RATES AN0 SHORT TRANSITION TIMES/ ELECTRORED 68PRR-108 LYSIS FOR LITHIUM AN0 FLUORINE IN GRAPHITE, USING A SLIT SCANNING TECHNIQUE/ PROTON REACTION ANA 68PRR-046 IUM-170 I/ CHARACTERIZATION OF ISOTOPE MATERIALS I DECAY SCHEMES / IRON-59 / BARIUM-140 I SAMARIUM-I51 I R 68A-08-060 TkEORY AN0 PRACTICE OF LIQUID SCINTILLATION CCUNTINGl 68PRR-117 BO NUCLEIC ACIDS I TRNA I/ COMPUTER PROCESSING OF LIQUID SCINTILLATION COUNTING DAT4 IN THE ANALYSIS OF TR 68A-04-01E TION 6Y USE OF TRITON X-LOO IN AN ORGANIC SYSTEM/ LIQUIO SCINTILLATION COUNTING OF WEAK BETA EMITTERS IN A 68A-08-02G QUEOUS SOLUTION USING TRITON X-lOO/ LIQUID SCINTILLATION COUNTING OF UEAK BETA EMITTERS IN A 6ePRR-045 OEVICF FOR SAWPLING GASES C@NTAINED IN SEALED METAL TUBES/ 68A-02-01C / FLUrlRlDE / DOTASSIUM CkLORIOE I OXYGEN I PYCNOMETER / SEALED TUBE OISSOLUTION I THORIUM / URANIUM NITRI 688-12-02 DIOISOTOPIC LIGHT SOURCE/ LNALYTICAL ~PPLICLTIONS OF THE SECONDARY EFFECTS OF RADIATION - PRECISION PHOTOM 68PRR-031 1ZE DISTRIBUTIOY OF PARTICLES FROM 10 TO 2000 MICRONS BY SEDIMENTATION ANALYSIS/ PARTICLE S 68PRR-007 PROSPECTS AN0 PRORLEMS FCR ACTIVATION ANALYSIS OF OCEAN SEDIMENTS/ 6RPRR-104 AN EVALUATION OF THE PERFORMANCF OF TYE NITRATF SELECTIVE ELECTRODE/ 68PRR-026 PE9FORM4NCE CHARACTERISTICS OF ION SFLECT IVE ELECTRODES/ 68PRR-120 138

EVALUATICN OF THE PERFORMANCE OF ION SELECTIVE ELECTRODES I ORION SULFIDE ELECTRODE I/ 6P4-02-09 S I AMMONIUY AZIDE / CALCIUM - GOLD ALLOY / GERMANIUM-73 ZELENIOE / GERMPNIIJY-73 TELLURIDE / NICKEL-54 - A 6ap-09 DETERMINATION flF TRANSFER RIB0 NUCLEIC PCID/ A SEMIAUTCMATEO FILTER PAPER DISK TECHNIQUE FOR THE 68PRR-003 ES IN HELIUM-3 ACTIVATION ANALYSIS/ RAPID CALCULATION OF SENSITlVITlESt INTERFEKEI'lCES1 AN0 OPTIMUM R7Y?bRD 6XPRR-030 UPS/ METHOD FOR SEPARATING MEMBERS OF ACTIIUIDF AND LANTHANIDE GRO hEPFR-l2O SEPARATION AND CONCENTRATION STUDIES/ 684-02-05 NTS/ NEW EXTRACTION CtROMATOGCAPHIC METHO3 FOR THE RAPID SEPARATION OF AMERICIUY FPOM OTHFR TRANSUQANIIIM E b8R-1 C-03 ION EXCHANGE/ NEW METHOD FOR THE RAPID SEPARATION OF BERKELIUY(1VI FROM CEHIUMIIVI 3Y AN 68~-io-ni ION EXCHANGE/ NEW METHOS FOR THF RADIO SEPARATICN OF BERKELIU~YIIVIFROM CERIUMIIVI F3Y AN 6?PRR-C24 SEPARATION OF CALIFORNIUM ( EINSTEINIUY I/ 6YA-02-07F L IGAN C EXC H AN 6F CHR OM4 TOGR A PHY / SEPAPATICN OF COMPGUNCS OF 3IOLOGICdL INTEREST BY bSA-04-CZB APPING WAVES IN STATIONARY ELECTRODE VOLTAMMETRYl ON THE SEPARATION OF HALF-WAVE POTENTIALS REQUIRED FOR R 6@A-01-14 APPING WAVES ltv STATIONARY ELECTROOE VOLTAMMETRYl ON THE SEPARATION CF HALF-WPVE PCTFNTIALS QEQUIREO FOR R 68PRR-C25 RAPID DTSTILLbTION ScP4Q4TION OF MICROGqAM OUANTITIES OF FLUllRIDt/ 6RPRR-018 HROMATOGRAPHY OY GELYAN ITLC-SA YEDIUMl SEPARATICN OF SIX COPTICDSTEROIDS BY THIN LAYFR C 6PPRR-075 SIN I/ COLUMN CHROMATOGRAPHY kITH ANTIMONY PENTA OXIDE I SEPARATION OF SOCIIUM / CHELEX-109 CATION EXCHANGE hRA-02-05A MACRCMOLECULAR SEPAR4TICNS PROGRAM/ 6 FA-04-01 GEL PERMEATION CHROMATOGRAPHY AS B SEPARATIONS TECHNIQUE/ ORR-1 C-l1C UM OF POLY ETHYLENE IMINE - CELLULOSE / MASS SPECTRUM OF SEPHADEX-G-75 / MASS SPECTRUM OF MEPCK SILICA GEL 6RA-02-OZF R.,1968 / MAY11969 / JUNE11968 / JULY,1968 / AUG..1968 / SEPT.rl968l ANALYTICAL CHEYISTRY RESEARCH AN0 DEV 6BPRR-060 SWITZERLANDI GERMANY, WEST GERYANYt NORWAY, AN0 ENGLANDI SEPT.2-30r1967/ REPORT OF CP9EIGN TRAVEL TO CZECH 6?3PRP-C47 , ITALY, GERMANY, THE NETHERLANDSt AND HARWELL, ENGLAND, SEPT.5-26.19t7/ REDCQT Oc FCREIGY TRlVFL TO CRAW OPPKR-C58 AMINO ACID SEQUENCE OF MOUSE HEYOGLnBIN/ 68A-04-03H SERVICE ANALYSES/ 6PB MASS SPECTROMETRY SERVICES/ 68P-ll-Cle SERVO CONTROLLED PIPETTERSl 68PRR-054 PUTOMATIC POTENTICMETRIC TITRATOR, VELOCITY SERVO, ORNL MODEL-Q-1728 BNO 'YODEL-0-172aA/ 68P9R-078 I/ MODIFICATION OF OVAL SET POINT VOLTAGE COMPAR4TOR I ORNL MODEL-Q-295C 6EA-01-15 MEN1 COMPUTER SYSTEM I POLAROGRAPHY / FLAME PHOTOMETRY / SIGNAL BVERAGING 4UTCYATION / CIRCUIT TESTS / 0.Y 686-01-21 UM FLUORIDE MIXTURES/ CONTAINMENT Or MOLTEN FLUORIDES 1'4 SILICA I. EFFECTS OF TEMPERATURES ON THE SPECTRU b8PRR-r)Ob MASS SPECTRUM OF SEPbADEX-G-75 / MASS SPECTRUM OF MERCK SILICA GEL G / MASS SPECTRUM gF CORNING POROUS GL 68A-OZ-CZF RECOVERY OF SILICON/ 68A-05-05C ROMATOGRAPHY ( GAS CPROMATOGRAPHIC OETECTCR SPECIFIC FOR SILICON I/ DERIVATIVE GAS CH 68A-02-01H I/ OETERYINATIDN OF SILICON IN CURIUM OXIDE ( DI CURIUY-244 TRI OXIOE 6@A-05-c15 L THI@ HYDANTCIN DERIVATIVES OF AMIYO ACIDS / TRI YETHYL SILYL PHENYL TH!O HYOPNTOIN DERIVATIVES OF &MINO 68A-02-ClO N ANALYSIS FOR LITHIUM AN0 FLUORINE IN GRAPHITE, USING A SLIT SCANNING TECHNIQUE/ PROTCN PEACTIO 6RPRR-046 CHARACTERIZATION OF TOBACCC SYOKE AND SMOKE CONCENSATESI 684-02-C3 CHARACTERIZATION CF TOBACCO SMOKE AN0 SMOKE COUDENSATESI 688- 10-1 1 CHARACTERIZ4TlON OF TOBACCO SMOKE AND SMOKE CONDENSATES/ 63A-02-03 CHARACTERIZATION OF TOBACCO SMOKE AN0 SMOKE CONDENSATES/ 688- 10-1 1 ORNL SMOKING MACHINE/ 68E-lO-11B CHRCMATOGRAPPY WITH ANTIMENY PENT4 OXIDE ( SEPAQATION OF SODIUM / CHELEX-100 CATION EXCHANGE RESIN I/ COLU 60A-02-05P INTERACTIONS OF HELIUM-3 PARTICLES WITH BORON. NITROGEN, SODIUM AND BERYLLIUM/ 68PRK-015 C MEASUREMENT OF COPPERIIII IN MOLTEN LITHIUM FLUORIDE - SCDIUM FLUORIDE - PCTASSIUY FLUORIDE / EFFECT OF 68A-03-021 LECTROCHEMISTRY OF TANTALUM IN MOLTEN LITHIUM FLUORIOE - SGDIUM FLUORIDE - POTASSlUY FLIJORIOE / ELCCTROCHE 6aA-03-021 OF OXIDE ANC hYDROXIOE IMPURITIES IN LITHIUY FLUORIDE - SODIUM FLUORIDE POTASSIUM FLUORIDE MELTS ON VOLTA 6RA-03-'221 AT OR / SOLI0 STATE CCXTROLLED POTENTIAL COULCMETRIC TlTR 6PA-Ol-Cl LAMTHINIOE HYDROXIDE SOLS/ 6SA-07-ClA SPECTROPHOTOMETRIC STUDIES OF SOLUTE SPECIES IN MOLTEN FLUORIDE MEOIAI 6RPRR-124 LTANEOUS ELFCTROCHEMICAL AN0 SPECTROPHOTOMETRIC STUDY OF SOLUTES IN MOLTEN FLUORIDE SbLTS [ ELECTQOCHEYlST bPA-03-CZ I AN0 ITS DETERMINATION 9Y BETA COUNTING/ CHROMATOGRAPHIC SOLVENT EXTRACTION 1SOLATII)N 0' BERKELTUY-249 FRO 68R-lO-O? AN0 ITS DETERMINATION BY BETA COUYTING/ CHROMATOGRAPHIC SOLVENT EXTRACTION ISOLITION OF BERKELIUM-240 FPfl 08PRR-013 NEUTRON ACTIVATION ANALYSIS WITH A CALIFORNIUM-252 SOURCE/ 6nA-08-01 C ATION - PRECISION PHOTOMETRY CSING A RADIOISOTOPIC LIGHT SOURCE/ AhALYTlCbL APPLICATIONS OF THE SECONDARY h8PRR-031 SPARK SOURCE MASS SPECTROMETRY1 68A-06-01 NEUTRON ACTIVATICN ANPLYSIS WITH CALIFORNIUP-252 SOURCES/ 68PRR-113 TlNGl SOURCES OF CONTAMINATION DURING ELECTRON BEAM MEL 6PPRR-057 TINGl SOURCES OF CONTdMINATION DURING ELECTRON BEAP MEL 68PRR-088 SPARK SOURCE MASS SPECTROMETRY/ 6e4-06-01 PMENT CENTER ACTIVITIES/ SPECIAL ANALYTICAL PSSISTANCE FOR ISOTOPES OEVELO 68A-08-06G PLANNED USE WITH SPECIPL INTERFPCES/ h4A-01-21R SPECTROPHOTOMETRIC STUDIES OF SOLUTE .SPECIES IN MOLTEN FLUORIDE MEDIA/ 68FRR-124 VATIVE GAS CHROMATOGRAPHY I GAS CHROMATOGRAPHIC DETECTOR SPECIFIC FOR SILICON I/ DER1 o8A-02-01H TlON METAL IONS IN MOLTEN FLUORIDE SOLlJTION [ ABSORPTION SPECTRA CF IRON(IIIr NICKEL(III1 CHROMIUM1 111. AN t PA-03-02G N FLUORIOE SOLUTION/ ABSORPTION SPECTRA OF SEVERAL TRANSITION METAL IONS IN MOLTE 6ePRR-123 AND CHROMIUM(1III IN MOLTEN FLUORIDE SALTS I/ ABSORPTION SPECTRA OF SEVERAL 3C TRANSITION METAL IONS IN MO 68P-03-02G IRRbDlbT IONS/ STANDARD GAMMA-RAY SPECTRA OF THE ELEMENTS FOLLOWING 14-MEV NEUTRON 68PR R- 121 M(IV1 IN MOLTEN LITHIUM FLUORIDE - BERYLLIUM FLUORIDE I/ SPECTRAL STUOIES OF URPNIUM(V1 AND URAYIUMIVII IN 684-03-02E X-RAY AN0 OPTICAL SPECTROCHEMISTRY/ 684-05 BEAM SPLITTER FOR USE IN CALIBRATING SPECTROGRAPHIC EMULSIONS/ 684-05-02 BEAM SPLITTER FOR USE IN CALIBRATING SPECTROGRAPHIC EMULSIONS/ 68PRR-C89 APPLICATIONS OF A BERYLLIUM WINDOW GERMANIUM - LITHIUM SPECTROMETER SYSTEM/ 68A-08-03C MASS SPECTROMETRIC DATA REDUCTION/ h@4-06-04 MASS SPECTROMETRY/ 68A-Ob SPARK SOURCE MLSS SPECTROMETRY/ 6ea-oc-ci b STUDY OF PARAMETERS THAT AFFECT ANALYTICAL ALPHA SPECTRCMETRYl t8A-08-02E SPECTROMETRY/ 688-11 MASS SPECTRCMETRYl 685-11-01 TRANSURANIUM MASS SPECTROMETRY/ 688-11-018 EMISSION SPECTROMETRY/ 685-11-02 INFRAXEO SPECTROMETRY/ 685-1 1-03 D I CARYOPHYLLENE / LIPIDS I/ NUCLEAR MAGNETIC RESONANCE SPECTROMETRY I CINNAMYLIDENINDENE / 01 PHENYL BEN 686-11-04 TS OF THE MSRE/ MEASUREMENT BY GERMANIUM - LITHIUM GBMMA SPECTROMETRY OF FISSION PRODUCTS DEPOSITED IN COM 68A-08-04C LOW RESOLUTI@N MASS SPECTRCMETRY OF ORGANIC COMPOUNDS/ 68A-Ot-CE GELMAN ITLC-SP MFCIUM / MASS SPECTRUM OF ALLMINA I/ MASS SPECTRCMETRY OF SUPSTANCES ISOLATED BY THIN LAYER 68A-D2-C2F CHROMATOGRAPHY I WICK-STICKS I/ INFRARED SPECTROMETRY OF SUSSTANCES ISOLATED BY THIN LAYER 684-02-026 S FROM THE ANION EXCHANGE CHRCMATOGRAPHY CF URINE ( MASS SPECTROMETRY OF URINE COMPONENTS I/ DESALTING OF 08A-04-03E MASS SPECTROMETRY SERVICES/ ~SB-ll-DlB GERFANIUM - LITHIUM DIODE GPMMA SPECTRCMETRY SYSTEC/ 6eA-Oe-C4€ MODEL IX FLAME SPECTROPHOTOMETER/ 68A-01-17 SPECTROPHOTOMETRIC DETERMINATION OF PLUTONIUYl 68A-OZ-C7I AZO AND PLUTONIUMlIIIlr f'LLITONILJM(1VI 4ND PLUTONIUM(VII/ SPECTROPHOTOMETRIC DETERMINATION OF TOTAL PLUTON1 bUPRR-OJR DE - POTASSIUM FLUORIDE I ELECTROCHEMICAL GENERATION AN0 SPECTROPHOTOMETRIC MEASUREMENT OF COPPER(II1 IN M o8A-03-02 I 139

RS FOR YOLTEN FLUORIDE SALTS ( DIAMOND WINDOkED CELL FOR SDECTROPHDTDMETRIC MEASUREYENTS OF MOLTFN FLUORID 68A-03-02F EFFECT OF GAMMA RADIATION 011 SPECTROFHOTCMETRIC METHODS FOR IFON/ 68A-08-07F CLTFN FLUGRICE MEDIA/ SPECTROPHCTCMETRIC STUGIES CF S3LUTE SPECIES IN M t8PRR-I24 NUP METAL ELECTRODES I/ SIYULTANEOUS ELFCTROCYEMICbL AND SPECTROPHOTGMFTQIC STUDY OF S!lLUTFS IN MOLTEN FLU 6eA-03-021 NIORIUN IN MIXTIl2ES OF FLUORIDE SALTS. SPECTROPHOTOMET3IC THIO CY4NATE METHOD/ 68PRR-CB2 ABSORPTION SPECTQGPVDTOMETRY OF ALPHA EMITTING MATERIALS/ 680- 10-1 2 FACILITY FOP SPECTROPHOTOMETRY CF PADIOACTIVE SAYDLESl 60A-03-020 X-RAY S PEC TR OSC OPY / 6BA-05-01 BETWEEN 173-le5 RFGION/ NUCLEAQ SPECTRDSC@PY IN THE NEUTRGY DEFICIENT MASS NUMBER 6t?A-De-D3D ASS 7935 / MASS SPECTRUM OF GFLMAN ITLC-SA MEDIIJM / H4SS SPECTRUM OF ALUMINA )I MASS SPECTROMETRY OF SUBST 68A-02-D2F PHADEX-G-75 / YASS SPECTRUM OF MERCK ClLlCA GEL G / MASS SPECTRUM OF CGRAING POSOUS GLASS 7935 / MASS SPEC 68A-02-02F EL G / M4SS SPECTPUM CF CORNING P'3ROUS GLASS 7935 / MASS SPECTRUY OF GELYAN ITLC-SA '4EOIUM / MASS SPECTRUM 68A-02-02F MINE - CELLULCSE / MASS SPFCTRUM OF SEPHAOEX-G-75 / MASS SPECTRUY CF MEQCK SILICA GEL G / MASS SPECTRUM OF 68A-02-02F FTRA FLlJORO BERYLLATE/ SPECTRUM CF MOLYRDENUM(III1 FLUORIDE IN LITHIUP T 6BA-03-02H PHY I MASS SPECTQUM OF POLY TETPA FLUCRO ETHYLENE / MASS SDFCTQUP CF POLY ETHYLENE IMINE - CELLULOSE / MAS 6aA-DZ-CZF SUQST4NCES ISOLATED BY THIN LAYER CHROMATOGRAPHY I MASS SPFCTRUM OF POLY TETPA FLUOR9 ETYYLENE / MASS SDE 68A-OZ-OZF MASS SPECTRUM OF POLY ETI-YLENE IMINE - CELLULCSE / FASS SFECTRUM CF SEPHADEX-G-75 / x1ASS SPECTRUM OF MERC 686-02-D7F N FLUrlRICFS IN SILICA I. EFFECTS OF TEMPERATURES ON THE SPECTRUM CF URANIUMl4+1 IN MOLTEN BERYLLIUM FLUOR 6ePRR-006 TION IN REMOTE FACILlTlES OF GNEVEN FLUX/ AIR FLD4TING SPHERE FCR HOMOGENECUS PHOTON AND NEUTRON IRRADIA 68A-08-ClA ULSIONS/ BEAX SPLITTER FOR USE IN CALIBRATING SPECTROGRAPHIC FM 60A-05-02 ULSIONSl BEAM SPLITTER FOR USE IN CALIRRATING SPECTROGRAPHIC EM 6RPRR-Ce9 2 A C ICL Y S I 5 0 F P. A 0 I AT I ON S A F E G U A RD SPRAY S 0 LUT I GPI S / 60A-08-07A RAOIATICY 4ND THERMAL STARILITY OF SPRAYS/ 68PPR-125 PAL ACIDS/ STABILITY OF SOME INERT METALS IN IRRADIATFD MINF 68A-08-07D QADIATION AND THERMAL STABILITY OF SPQAYSI 69PQR-125 ING 14-MEV NEUTQGN IRRADIATIONS/ STANDARD GAMM4-RAY SPECTRA OF THE ELEMENTS FOLLOW 68PRR-121 ORATORY SUPERVISW - A STATUS QEPCRTI STAVDARD REFERENCE MATERIALS AS VIEYFC RY THF LA0 68PRR-034 RADIOACTIVITY STANDARDS/ 6!3A-08-C6C AVAILASILITY OF STANDARDS FOR C3MMGN RL3IOUUCLIOES/ 68PRR-028 P RESOLLlTI(?N OF SIMPLE, REVEPSIRL5. OVERLAPPING WAVES IN STATIONARY ELECTROGE VOLTAi4METRYI ON THE SFPARATI 6RA-01-14 R RESGLUTIOU OF SIMPLFI REVERSIBLE, OVERLAPPING WAVES IN STATIONARY ELECTRODE VOLTAYYETRY/ ON THE SEPPRATI 68PRR-025 EYISTRY DIVISIGN, JULY-SEPT.91?67/ STATISTICAL QUALITY CCNTPGL REPORT; ANALYTICAL CH 68PRR-039 EMISTPY DIVISIONt OCT.-DEC.. 1967/ STATISTICAL QUALITY COUTROL REFOQT. ANALYTICAL CH 6PPRR-C4C EMISTRY DIVISION. JAN.-MAR..1568/ STPTISTICAL QUALITY CONTROL REPORT, ANALYTICAL CH 6RPRR-041 EMISTFY QIVISIONI APR.-JUNE11?68/ STATISTICAL QUALITY CONTROL REPORT, ANALYTICAL CH 68PRR-042 USE OF STATISTICAL TECHNIQUES IN FLAME PHGTOMETRYl 684-01-18 PREVIOUS STATUS OF PRObLEMl 6BA-D5-G5A NCE MATERIALS PS VIEWFD BY THE LAQORATORY SUPERVISOR - A STATUS REPORT/ STANDARD REFFRE 68?RR-C34 ANALYSES I FLUORESCENCE OF STEROIDS / PHOSPHORESCENCE OF STEROIDS I/ STEROIDS ( GELMAN ITLC-SA YEDIUY / 00 68A-02-02E ITLC-SA MEDIUM I 00CY FLUIDS ANALYSES / FLUORESCENCE OF STEROIDS / PHOSPHORESCENCE OF STEROIDS )I STEROID 68A-02-C2E LUORESCENCE OF STFPOIDS / PHOSPHORESCENCE OF STEPOIDS )/ STEROIDS ( GELMPN ITLC-SA YFCIllY / BODY FLUIUS AN 684-02-PZE EACTOR PRESSURE VESSFL/ STRESS ANALYSIS IN TAPERED TRANSITION JOINTS IN R 64TR-GI STRONTIUM-90, PRODUCT ANALYS IS GUIDE/ 66PRR-075 STRONTIUM-92. PR@CLICT ANALYSIS GUIDE/ 68PRR-074 CHLORPTE YECIA 111. RESnLUTIY OF THC ULTRAVIOLET 8hNO STRUCTURE - SGME CONCLUSIONS CONCERNING THE EXClT 68PRR-DC8 SUMYER STUDENT PROGRAMS/ 68D-14-05 npbi; I -- STUDENT TRAINEE PRCGRAM~ 6RD- 14-D5A E DILUTION - AMINO ACYLATIGVl DETERYINAT13N OF SURNANOMDLE QUANTITIE5 OF L AMINO ACIDS BY ISOTOP 6 OA- 04-0 1 L EDIUM / MASS SFECTRUM OF ALUMINA I/ MASS SPECTROMETRY OF SUSSTANCES ISOLATED RY THlU LAYER CHQGMATOGRAPHY 6 EA- 02- 02 F I WICK-STICKS I/ INFRARtD ZPECTROMETQY OF IUB>TANCES ISOLATED BY THIN LAYER CHQOMATOGRAPHY 68A-02-O2G AMINO ACID SU8STITUTIONSI 6BA-04-031 CONTROLLEC POTENTIAL CIFFERENTIAL DC POLAROGRAPHY V. SUPTRACTIVE POLARCGRAPHY/ bRPRR-C33 N OF THF PERCOQMANCE OF ICN SELECTIVE ELECTRODES t DklDN S'JLFIDE ELECTRODE I/ EV4LUfiTIO 68A-02-09 POLAROGQAPHY OF SULFUR 01 OXIDE I SULFITE 1 IN AQUEOUS HYDROFLUORIC ACID/ 68A-02-08C METHYL PhCSPHGRIC TRI PMIOE / 04RIUM PARA ETHYL BENZENE SULFONATE / ESTROLOLACTDNE / 2 BETA YETHYL 19 NOF 680-11-04 PCLARDGRIPHY OF ZIRCONIUM IN ACETONITQILE 4ND DI METHYL SULFOXIDE/ 68A-Dl-C7 ANTITATIVE FLCCTRODEPOSITIDN OF ACTINIDES FROM DI METHYL SULFOXIDE/ QU 68A-OR-020 LYYERS / 5 FURFURYL FUPFURYL ALCOHgL / DEUTERD 01 METHYL SULFOXIDE / HEXA METHYL PH@SPHORIC TRI AYIOE / RA 6PR-11-04 IC ACID/ PDLARDGAAPHY OF SULFUR DI OXIDE I SULFITE I IN AQUEOUS HYOROFLUOR 604-02-O8C 8/ ANALYTICAL CHEMISTRY RESEARCH AN0 DEVELOPMENT MONTHLY SUMMARY - NOV.11967 / OEC.91967 I JAN.rl968 / FER 6BPRR-060 SUMMER STUDENT PROGRAMS/ 680- 14-05 STANDARD PEFEQEYCE MATERIALS AS VIEWED BY THE LABORATORY SUPERVISOR - A STATUS REPORT/ 68PRR-034 ABORAT@PY/ RESEARCH ANC SUPPORT ACTIVITIES IN THC TRANSUR4NIlJM RESEARCH L 68A-02-07 ENTIALS OF TI-E LPNTHANIDES/ SURFACE ICNIZATION 111. THE FIRST IOP~IZATIDNPOT 68PRR-016 IOUS GXYGEN PRESSURES/ SURFACE ICNIZATION OF URANIlJMlIVl FLUORIDE AT VAR CRA-06-C3A SURFACE ION1Z AT ION STUDIES/ 6epl-06-w AIR OUALITY SURVEY I 68A-02-06 LITERATURE SURVEY/ 680-10-11A APHY I BODY FLUIDS ANALYSES PROGRAM )I POLAROGRLPHIC SURVEY OF EIOCHEMICILS I DIFFERENTIAL OC PULAQDGR 60A-Dl-C8 1967/ REPORT GF FOREIGN TRAVEL TO CZECHOSLOVAKIAI ITALY, SklTZERLANO. GERMANY, WEST GERMANY, NORWAY, AND E 63PRR-047 JULY-10-31.1SfB/ REPCRT CF FOREIGN TRAVEL TO ENGLAND, SWITZERLANOI ITALY, CERMANY, AN0 THF NFTHERLANDS. 68PRR-C71 MISTRY 1'4 NUCLEAR TECHNOLOGY/ SYNOPSIS OF ELEVFNTH CONFERENCE ON ANALYTICAL CHE 68PPR-032 F SOLUTES IN MOLTEN FLUORIDE SALTS ( ELECTROCHEMISTRY OF TANTALUM Ih MOLTEN LITHIUM FLUORIDE - SODIUM FLU0 68A-03-021 SELl STRESS ANbLYSIS IN TAPERED TRANSITION JCINTS IN REACTOR PRESSURE VES 68TR-C1 NEUTRON GENERPTOR TPRGET DEVELOPMENT PROGRAM/ 68A-08-D5C ONUCLIDES COBALT-57r MOLYBDENUM-99 - TECHNETIUM-~~MI AND TECHNETIUM-99MI INTERLABORATORY COMPARISON OF MEA 68A-08-03A HALF-LIFE MEASUREMENTS I TECHNET IUM-99M I / 688-08-D6E UREMENTS OF THE RACIDNUCLIDES COBALT-57. HOLYEOENUM-99 - TECHNETIUM-~~MI AN0 TECkNETIUM-99NI INTERLASORATO 68A-Oe-C38 TECHNICAL ASSISTANCE/ 68A- 0 8-06 A lNFORPATION PACKACES SUBMITTED TO THE DIVISION OF TECHNICAL INFDRMATICN EXTENSIDHI 68A-01-12 IENTS I/ EUTROPHIC WATER SYSTEMS I PHOSPHATE / NlTRbTE / TECHNICON AUTOANALYZER I HYDROPONIC BEDS / ALGAL 6 B A-0 2-,04 8 F ELEVENTH CONFERENCE ON ANALYTICAL CHEMISTRY IN NUCLEAR TECHNOLOGY/ SYNOPSIS 0 68PRR-032 / LIQUID ION EXCHANGERS I/ POLY TETRA ELUCRO ETHYLENE I TEFLON I AS AN ADSPRBENT ( 01 2 ETHYL HEXYL ORTHO 688-02-028 PHIC LATA/ EVALUATICN OF VERTICAL ORIFICE RAPID TEFLON D.C.E. FOR OETbINING FUNDAMENTAL POLARDGRA 68A-DZ-CeA IUM IN 1 MOLAR HYOROFLUDRIC ACID WITH A VERTICAL ORIFICE TEFLON DROPPING YERCURY ELECTRODE/ RAPID POLAROGR 68P-02-08B POLAROGRAPHIC STUDIES WITH THE TEFLON DROPPING YERCURY ELECTRODE I O.M.E. I/ 68A-02-08 CIUM - GOLD ALLOY / GERMANIUP-73 SELENIDE / GERMAYIUY-73 TELLURIDE / NICKEL-64 - ALUWINUM ALLOY / NICKEL-6 68A-OS CONTAINMENT CIF MCLTEN FLUORIDES IN SILICA I. EFFECTS OF TEMPERATURES ON THE SPECTRUM OF URANIUM(4+1 IN MO 6RPRR-006 LIGANC EXCHANGE CHROMATOGRAPHY/ TERMINAL NUCLEOSIOE ASSAY OF RIBD NUCLEIC ACID BY 688.-04-011

/--- L IGAND EXCHANGE CHROMATOGRAPHY/ TERYINbL NUCLEDSIOE ASSAY rJF RIBO NUCLEIC ACID BY 6 BP RC09R- OS BY LIGAND EXCVANGE CHROMATCGRAPHYl ASSAY OF 3/ TERMINAL hUCLEGSIOES OF TRANSFEP 2100 NUCLEIC ACI 68PRR-085 NUCLEAR METHODS FOR EXTRA TERRFSTRIPL ANALYSIS/ 68PRR-116 ENZFNE SULFONATE / ESTROLGLACTGNE / 2 BETA METHYL 19 NflR TEST0 LOLACTDNE / 2 ALPHA METHYL ESTRA 4 FNE 3-17 680-11-04 140

FLAME PHOTOYCTRY / SIGNAL IVERAGING AUTCMATION / CIRCUIT TESTS / O.M.E. / ENSEMBLE AVERAGING )I ANALYTICAL 6R4-01-21 ES IN RELATED CRAFT TRAINING/ VALIDITY OF SOME TESTS OF INT'LLECTUAL ABILITY FOR PREDICTING GrAO 68PRR-Or)S Q ELFCTRICAL AND ELECTROCHEMICAL TESTS CF PERFCIRMANCE CF POLIROGKAPHS/ hen-01-05 AL GAS ANPLYZER )I ANALYSIS CF PURGE GAS FROM IN RFACTOF TESTS OF REACTO? FUEL ELEYENTS ( MONOPPLF 600 RES 68A-03-C3A TASSIUM NICKELIIV) PAPA PFR IPCATE 1/2 hbTER / PflTASSIUY TETRA CYANO NICKELATF(I1) / TETRA KIS TRI PHV'dVL 688-09 SPECTPUM OF P~LYBOENIJM(III) FLUCRIDF IN LITHIUM TETRA FLUORO @ERYLLATC/ ~~P-O~-P?H STUDIES OF URANIUM(V) AND URANIUM(V1) IN MOLTEN LITHIUM TETRA FLUORG BERYLLATE I OISPROPORTIONATION OF UR 68A-03-02F

RY HYDROFLUORINATION~~ ( OETEPWINATION OF OXIDE IN LITHIUM TETRA FLUORO BERYLLATF AN0 IN LITHIUM FLUORIDE - 68A-07-016 GRAVIMETRIC DETERMINATION OF TETRA FLUORO BORATE WITH NITRONl t 8R-10-C5 TED 3Y THIN LLYER CMRCMATOGRAPI'Y ( MASS SPECTRUM OF POLY TETRA FLUCRO ETHYLENE I MASS SPECTRUM OF POLY ETH 6flA-02-CZF PHOSPHORIC ACID / HOFHP / LIQUID ION EXCHANGERS I/ POLY TETRA FLUCRD ETHYLENE < TEFLON I AS AN ADSORGENT 6P4-02-028 IODATE 112 WATER / POTASSIUM TETRA CYANO NICKELATE(I1) 1 TETRA KIS TRI PHENYL PHOSPHITE NICKEL(0) l/ INORG 688-05 RICIUM / EUROPIUM / HEXA FLUCRO ACETYL ACETONE / 2,2,6,6 TETRA METHYL 3,5 HEPTANE DIOUE )I PREPARATION mn 681-02-071; ING/ THECRY AND PRACTICE OF LIQUI0 SCINTILLATIDY COUNT 6QPRR-117 OIOQCTIVE MSRE FUEL BY HYORDGEN REDUCTION ( ABS@RPTION - THERMAL CCNDUCTIVITY YEASUREVENT OF HYOROGEY FLU0 h5A-03-018 NEW NUCLEAR DATA ( GAMMA-PAY ENEPGIES I TYERMAL NEUTRON CROSS SECTIONS )I 66A-OP-C38 RADIATION AYC THE'IMAL STARILITY CF SPQAYSI 6PPRR-125 THEPMOGPAVIMET9IC ANALYSIS OF THORIUM IODATE/ hRB-10-C4 GRADUPTE THESIS RESEARCH PROGRAMS/ 6 80- 14-03 HI THIN FILM MERCURY ELECTRODE VOLTAMMETRY OF RJSMUT 6RB-10-10 THIN LAYER CHROMATOGRAPHY/ 698-02-02 THIN LAYER CHRUMATCEPAPHY/ 6RA-02-C3B F ALUMINA )I MASS SPECTROMETRY OF SUBSTANCES ISOLATED 6Y THIN LAYER CHROMATGGRAPHY ( MASS S?ECTRUM CIF POLY 68A-fl?-C2F IYFRAhFO SPECTRDMETRY CIF SUBSTANCES ISOLATED BY THIN LAYER CHROMATCGRAPHY ( WICK-STICKS I/ 686-02-02G M/ SEPARATICN OF SIX CORTICOSTEROIDS BY THIN LAYER CHROMATCGRAPHY SN GELYAN ITLC-SA YEOIU 68PRR-076 D 8ASESI NUCLEOSIDESI AND NUCLEOTIDES @Y TWO DIMENSIONAL THIN LAYER CHR@MATflGPAPHY ON POLY ETHYLENE IMINE 6qPRR-027 NATION OF CADMIUM IN PLUTONIUW ( AMMONILM PYRROLIOINE 01 THIO CARBlMATE ( APOC 1 I/ OtTFPYI 684-09-043 IOBIUM IN MIXTURES OF FLUORIDE SALTS, SPECTROPHOTOMETRIC THIO CYANATE YETH3OI N 68PRR-032 DIN DERIVATIVES OF AMINfl ACIDS / TRI METHYL SILYL PHENYL THIO HYDANTOIN OERIV4TIVES OF AMINO ACIDS )I RIOY 68A-02-01D L APPLICATIONS ( FREE FATTY ACIDS / AMINO ACIDS / PHENYL THIO HYDANTOIN DERIVATIVES CF AMINO ACIDS / TRI Y 68P-02-PlO LORIDE / OXYGEN / PYCNOMETER / SEALED TUBE DISSOLUTION I THORIUM / URANIUM NITRIDE I/ GENERAL ANALYSES LA@ 6eR-12-02 THERMOGQAVIMFTPIC ANALYSIS OF THORIUM IODATE/ ~~B-Ic-c~ I/ QUILITY CONTROL ( hAOICPHARMACEUTICALS / CAR8ON-14 / THULIUM-168 / THULIUM-170 / ThULIUM-171 / TRITlUI* 6P?\-08-C6B M / RUBIDIUM-84 / IODINE-129 / IODINE-130 / YTTRIUM-?! / THIJLIUM-170 )I CHARACTFQIZATION OF ISLITOPE MATER1 ~BA-c)~-o~o NTROL I RADIOPHARMACEUTICALS / CARBON-14 / THULIUM-168 I THULIUM-170 / THULIUY-!71 / TQITIUY I/ QUALITY CU 68A-G?-069 HARMACEUTICALS / CARBON-14 / THULIUP-160 / THULIUM-170 I THULIUM-171 / TRITIUM I/ QUALITY CONTROL I RADIOP 684-08-068 DESIGN OF TIME AVERAGING AND TIYF DERIVATIVE CIRCUITS FOR 0 68A-01-10 r. POLAROGRAPHSI~~ OC POLAROGRAPH AND CRNL MUOFL-0-2942 POLAROGRAPHIC DROP TIME CONTROLLER/ GRNL MODEL-0-2792 CONTROLLED POT 68A-01-09 POLPROGRAPHIC DROP TIME CCNTROLLER I MOCEL-8-2542/ 68PRR-C4S CFSIGN OF TIPE AVERAGING AN0 TIME DERIVATIVE CIQCUITS FOR OC POCAROG'7APHS/ 684-01-10 NEUTRON ACTIVPTION ANALYSIS OF BRAIN TISSUE FOR COPPER AVO MANGAi4ESE/ 68A-OP-01F NFU._.. TITRANT DELIVERY UNIT AN0 ELEVATOR/ 6PA-Dl-C36 MICQO TITQATION OF PLUTONIUY/ 684-02-07C INSTRUYENT FOR END POINT OETECTIOY IN BIPOTENTIOMETRIC TITRATIONS/ 68A-01-11 SOLI0 STATE CONTROLLED POTENTIAL COULOMETRIC TIT9AT OR/ 484-01-Cl AUTOVATIC POTENTIOMETRIC TITRATOR/ 68PRR-052 ON OF THE ORNL MODEL-Q-2564 PIGH SENSITIVITY COULOMETRIC TITRATOR/ YO0 IFIC 4T I 68PRR-048 HIGH SENSITIVITY COULOMETRIC TITRATOR / MODEL-Q-2564/ 6RPRR-053 TO THE HIGH SENSITIVITY CONTROLLED POTENTIAL COULOMETRIC TITRATOR ( ORNL YCOEL-Q-2564 I/ MODIFICATIO'IS 68A-01-02 ORNL MGOEL-Q-2564/ COULOMETRIC TITRATOR. CONTROLLED POTENT I AL I HIGH SEN SIT1VI TY, bflPRR-C77 ODEL-Q-1728Al AUTdMATIC POTENT1 OMETRIC TITRATOR, VELCCITY SFRVOI ORNL YODEL-Q-1723 AN0 Y 68pRR-C78 TITRIMETRIC OETERPIhATION LIF AWERICIUM/ 686-02-078 CHARACTERIZATION OF TJBACCC SMOKE AN0 SMOKE COYDENSATESl t8A-02-03 CHARACTERIZATION OF TOBACCO SMOKC AND SMOKE COUCENSATESI 688-10-1 1 ) AN0 PLUTONIUMfVI)/ SPECTRDPMOTCMETRIC DETERMINATION OF TOTAL PLUTONIUM - CBSERVATI9NS ON THE REACTIflNS R 68PRR-038 DETERMINATION OF TOTAL REDUCING POWER OF RADIOACTIVE MSRE SALTS/ brjA-03-01C AMANITA TOXINS (GALERINA MARGINATP )I 684-02-021) TRAT ICNl MISCELLANEOUS TRACE OETERMINATICNS INVOLVING CHEMICIL PRECUNCEN 68A-05-C4 CHEYICAL PRECONCENTRATION OF TRACE ELEMENTS IN BONE ASH/ 68A-05-03 TRACE ELEMENTS IN OQUGSI 68A-08-01E FORENSIC APPLICATION OF TRACE ELEMENTS IN HAIR/ 6RPRR-002 FLUORIDE MIXTURES/ DETERMINATION OF TRACES OF RISMUTH IN LITHIUM FLUORIDE - BERYLLILJY 6 8A- 0 5- 04C R FREE PROCEDURE )I OFTERMINATION OF TRACES OF RARE EARTH ELEMENTS IN BISMUTH ( CAPRIE 684-05-044 ORAU STUDENT TRAINEE PROGRAM/ 680-14-056, ELLECTUAL ABILITY FOR PRECIClING GRADES IN RELATED CRAFT T RBIN I NG/ VALIDITY OF SOME TESTS OF INT 68PRR-CO5 TED FILTER PAPER DISK TECHNIPUE FOR THE DETERMINATION OF TRANSFER RIBC NUCLEIC ACID/ A SEMIAUTCMA 6PPRR-003 OETERMINATICN OF METHIONINE ACCEPTING TQANSFER RIBO NUCLEIC ACID ( METHIONINE TRNA )I 68A-04-Cl 8 KINETICS OF AMINO ACYLATION flF TRANSFER RIBC hUCLEIC ACID ( TRNA I/ 68A-04-01F ETHOD FOR OPTIMIZING CONDITIONS FOR THE DETERMINATION OF TRANSFER RIB0 NUCLEIC ACID I TRNA )I A FRACTIONAL 68A-04-01C ES / NUCLEOTIDES / NUCLEIC ACID SbSES I/ CONSTITUENTS OF TRANSFER RIBO NUCLEIC ACID I TRNA ) I POLY ETHYLE 68A-02-DPC OETERMIhATION OF TYROSINE ACCEPTING TRANSFER RIBO NUCLEIC ACID ( TYPOSINE TRNA )/ 68A-04-ClA CHNIPUE )I INSTRUMENTATION FOR ANALYTICAL BIOCHEMISTRY I TRANSFER RIRCl NUCLEIC ACIDS / TRANSFER RNA / FILT 688-01-19 AUTOMATED DETERMINATION OF TRANSFER RIBC NUCLEIC ACIDS ( TRNA )I 68A-04-010 CHEMICAL ANALYSIS OF TRANSFER RIB0 NUCLEIC ACIDS I TRNA )I 6@A-O4-C1 H OF LIQUID SCINTILLAT13N COUNTING DATA IN THE ANALYSIS OF TRANSFER RIB0 NUCLEIC ACIDS ( TRNA I/ TOMPUTtQ PR 6RA-04-01E ROMATOGRAPHYI ASSAY OF 3/ TERMINAL NUCLEOSIDES OF TRANSFER RIB@ NUCLEIC ACIDS BY LIGAND EXCHANGE CH 6RPRR-OR5 ANALYTICAL BICCMEMISTRY ( TRANSFER RIBO NUCLEIC ACIDS / TRANSFER RNA / FILTER PAPER DISK TECHNIQUE JI INS 684-01-19 STRESS ANALYSIS IN TAPERED TRANSIlICh JOINTS IN REACTOR PRESSURE VESSFLl 69TP-01 OLTEN FLUORIDE SALTS )I ABSORPTION SPECTRA OF SEVERAL 30 TRANSITICN METAL ICNS IN MOLTEN FLUORIDE SOLUTION 6 8A-03-02 G I ABSORPTION SPECTRA OF SEVERAL TRANSITION METAL IONS IN MOLTEN FLUORIrE SOLUTION 68PRR-123 UORIOE - ZIRCONIUM FLUCKIOE 4T FAST SCAN RATES AN0 SHOPT TRANSITIOh TIMES/ ELECTROREOUCTION OF URANIUMIIV) 68PRP-108 NIUM(II1) IN RADIOACTIVE MOLTEN SALT REACTOR FUEL/ A TRANSPIRATION METHOC FOR THE DETERMINATION OF URA 68PRR-087 METHOD FOR THE RAPID SEPARATION OF AMERICIUM FROM OTHER TRANSURANIUM ELEMENTS/ YEW EXTRACTION CHROMATOGRA 688- 10-133 / OXYGEN - TO - METAL RATIO / PLUTONIA / PROTACTINIUM / TRANSURANIUM ELEYENTS / URANIA / ZI9CONIA I/ HIGH 6PB-12-01 TRANSURANIUM MASS SPECTROMETRY/ tflR-11-C1 A RESEARCH AN0 SUPPORT ACTIVITIES IN THE TRANSURANIUM RESEARCH LABORATORY/ 684-02-07 REPCRT OF FOREIGN TRAVEL TO AUSTRALIAr FEB.l-MAR.7.105BI 68PRR-044 , NORWAY, AN0 ENCLANO, SEPT.2-30.lS67/ REPORT OF FOREIGN TRAVEL TO CZECHOSLOVAKIAI ITALY, SWITZFRLANDI GER 68PRR-047 EECE. AUG.29-OCT.8rlS67/ REPORT OF FOREIGN TRAVEL TO CZECHOSLOVAKIA, YUGOSLAVIA, AUSTRIA1 GR 68PRR-043 NO THE NETHEPLdNOSt JULY-10-31.1960/ REPORT OF FOREIGN TRAVEL TO ENGLAND, SUITZERLANO, ITALY, GERKANY, A 68PRR-C71 AN0 HARUELL, ENGLAND, SEPT.5-2691967/ REPORT OF FOREIGN TRAVEL TO FRANCE, ITALY, GERiqPNY, THE NETHERLANDS 68PRR-058 URCESl TQENO IN ATOMIC POWER GENERATIIN AN0 URANIUM RES0 68TR-02 L / OEUTERO 01 METHYL SULFOXIDE / YEXA METMYL PHOSPHORIC TRI AMIDE / BARIUM PARA ETHYL BENZENE SULFCNATE / 688-11-04 14 1

INATION OF THE METHYL ESTERS OF BUTYL PHOSPHORIC ACIDS ( TQI METHYL PHOSPHATE / DI METHYL BUTYL PHOSPHATE 6RA-02-01E IDS / PHENYL THIO HYDANTOIN DERIVATIVES OF AMINO ACIDS / TRI METHYL SlLYL PHENYL THIO HYDANTOIN DERIVATIVE 68A-02-010 DETERMINATION CF SILICDN IN CURIUM OXIDE ( DI CURIUM-244 TRl OXIDE I/ 688-05-05 WATER I POTASSIUM TFTQA CYANC: NICKELATE(lI1 / TETRA KIS TRI PHENYL PHOSPHITE NICKEL(D1 )I INORGANIC PRFPA 6RA-09 / CARBON-14 / THULIUM-168 / THULIUM-170 / THULIUM-171 / TRITIUM I/ QUALITY CONTROL ( RAOIODHAPYACFUTICALS h8A-08-068 CCUNTING OF WEPK BFTA EMITTERS IN AQUEOUS SOLUTION USING TRITON X-1001 LIQUID SCINTILLPTICN 6APRR-045 TING OF WFAK BETA EYITTERS IY AOUEOIJS SOLUTION 5Y USE OF TRITON X-100 IN AN OPGANIC SYSTEM/ LIQUID SCINTIL 6PA-CR-02G AUTOMATEG DETERMIYATION OF TRANSFER RISP NUCLEIC ACIDS ( TRNA I/ 68A-04-01D CHEMICAL ANALYSIS CF TRANSFER RI3O NUCLEIC ACIDS ( TKNA I/ 68A-04-01H ETICS OF AMINO ACYLATION OF TRANSFER RlRD NUCLEIC ACID ( TRNA I/ KIN 68A-04-CIF TYROSINE ACCEPTING TRANSFER RIbO NlJCLElC ACID I TYROSINE TRNA )I OETE2MfNATION OF 6BA-04-01A IONINE ACCEPTING TRANSFER Rreo 'IUCLEIC ACID ( METHIONINE TRNA )I OFTEPMINATION OF METH 68A-04-018 NS FOR THE QETERMINATION OF TFANSCER RIP0 NUCLEIC ACID ( TRNA )/ A FFACTIDYAL FACTORIAL METHOD FOR DPTIYIZ 6UA-04-ClC NG DATA IN TkE ANALYSIS OF TRANSFER PIRO NUCLEIC ACIDS ( TRNA )I CCMPUTER ORCCESSING 7F L1b)UID SCIYTILLATI 6 84- 04-0 1 E ID BASES I/ CONSTITUENTS CF TRANSFER RIBG NUCLEIC ACID ( TRNA ) ( POLY ETHYLENE IMIYE - CELLULOSE / NllCLEfl 68A-02-02C PETA METHYL ESTEA 4 ENE 3.17 DIONE / OI eQOMO FLUOPENE / TRUXENE / UREA / VARCJM / FAPI I FURFURAL / HIPPU 688-11-04 RIDE / PCTASSIUM Ct-LOPIOE / CXYGFN / PYCNCMETER / SEALED TUBE DISSOLUTION / THORIUM / URAYIUM NITRIDE I/ G 685-12-02 OFVICE FOR SPMPLING GASES COlLTAINED IN SEALED METAL TUBES/ 6EA-02-01C YROSfPlE TRNA I/ OETERMINATICU OF TYROSINE lCCEPTlNG TRANSFER RISO NUCLEIC ACID ( T bBA-D4-G1A ATIOY OF TYROSINE ACCEPTING TRANSFE? RIB0 NUCLEIC ACID ( TYROSINE TRNA )I DFTE2YIY hBA-04-01A URANYL ICN IN PER CHLCRATE MEDIA 111. RESOLUTION OF THE ULTRAVIOLET BPNO STRUCTUQE - SOYE CONCLUSIONS CON 68PRR-CC8 DEVICE FOR THE UNATTENOED CONCENTRATICN SF S@LUTIONS/ 6AA-02-05C ORNL UNOERGRACUATE PROGRAM/ 68D-14-058 S PHOTON AND NEUTRON IRRAGICTION IN RC~OTEFACILITIES OF UNEVEN FLUX/ AIR FLOATING SPHERE FOP HOMOGEN€DU 68A-08-016 NEW TITRANT DELIVERY UNIT AND ELEVATOR/ 68A-0!-034 AT10 / PLUTONIA / PROTICTINILY / TXANSURANIUM ELEMENTS / URANIA / ZIRCONIA )I HIGH LEVEL ALPHA RAOIATIOY L 6RB- 12- C1 RAPID SCAN POLPROGRAPHIC OETFRMINATION OF URANIUM/ 6RP-10-09 PRFCISF OETEPMINATION OF URANIUM IN MSRE FUEL/ 68B- 1C- 14 TEFLON DROPPING MERCURY ELtCTRDOE/ PADID POLAROGRAPHY OF UQAYIUM IN 1 WtOL4R HYDROFLUQRIC ACID WITH A VERT1 6RA-02-085 XYGEN / PYCNOYETER / SEALED TUBE 91SSOLUTIPN / THORIUM / URANIUM NITRIDE )/ GENERAL ANALYSES LABORATOQY ( 68B-12-02 TREND IY ATOMIC POWER GENERATION AND URANIUM RFSOlJRCESl 68TR-G2 PRECISE DETERMINATION OF URbNIUM-235I bRA-OE-C4A VEL/ A TRANSPIRATION METHOD FOR THE OETERMINATIOV OF URANIUM(II1) IN RADIPACTIVE MOLTEN SALT REACTOR F tbPRR-OP7 REMENT OF HYDROGEN FLUOPIOE IN GAStS )/ DETERMINATION OF URANIUM(II1) IY RADICACTIVE MSRE FUEL BY HYDROGEN 6PA-03-018 65.6-29.4-5.0 MOLE PERCENT ) EVIDENCE FOR AOSOHPTIOY OF UKANIUM(IV I ELECTRCCHEMICAL REOUCTION OF URANIUM CRPRR-022 SURFACE IONIZATION OF URANIUM(1V FLUORIOE AT VARIOUS OXYGEN PRESSURES/ 6RA-06-034 N LITHIIJM TETRA FLUilRG BFRYLLATE I DISPROPORTIONATIPN OF URANIUMIIV IN MOLTEN LITHIUM FLIJORIOE - RERYLLIU 68A-03-02E ADSDRPTIOY OF URANIUM( IV)/ ELECTROCHEMICAL REDUCTION OF URANIUM1 IV IN MOLTEN LITHIUM FLUORIDE - BERYLLIU 6RPRR-072 PN RATES AND StORT TRPNSITION TIMES/ ELECTROREDUCTION OF URANIUM(IV IN MOLTEN LITHIUM FLUORIDE - BERYLLIU 68PRR-108 LITHIUM TETRA FLUORO BERYLLATE AND IN LITHIUM FLUORIOE - URAN!UM(IV -233 FLUORIDE )I DETERMINATION OF OXln 68A-03-DlA IUM FLIJORIOE - EEPYLLIUM FLUORIDE I/ SPECTRAL STUDIES OF URANIUM(V) AND dRANlVH(VI) IN MOLTEN LITHIUY TETR 68A-03-O2E 500C/ DISP9CPC:RTIONATION OF ELECTROCHEMICALLY GENERATEO URANIUMlVl IN nOLTEN LITHIUM FLUORIDE - RERYLLIUM 6RA-03-02A 500CI OISPROPCRTIONATION OF ELECTRCCHEMICALLY GENEP.ATFD URANIUM(VI IN MOLTEN LITHIUM FLUORIDE - BERYLLIUM 68PRR-023 50OCI DISPROPCRTIONATION OF ELECTROCHEMICALLY GENERATEO URANIUM(V) IN MOLTEN LITHIUM FLUPRIDE - BERYLLIUM 68PRR-109 BERYLLIUM FLUORIDE I/ SPECTRIL STUDIES OF URANIUMIV) AND URANIUM(V1 IN MOLTEN LITHIUM TETRA FLUORO RERYLL 68A-07-02E IN SILICA I. EFFECTS OF TEMPEPATURES ON THE SPECTRUM OF URANIUM(4+ IN MOLTEN BERYLLIUM FLUORIDE - LITHIU 68PRR-CD6 CTURE - SCIME CCNCLUSIONS LONCERNING THE EXCITED STATE OF URANYL IOh AeSORPTION OF THE URANYL ION IN PER C 68PPR-CO8 RNING THE EXCITED STATE OF URAVYL ION/ ABSORPTION OF THE URANYL ION IN PER CHLORATE MEDIA Ill. RESOLUTION 68PRR-CC8 L ESTRA 4 €NE 3,17 DIONE IO1 BRCM3 FLUORENE I T?UX€NE / UREA I VARCUM / PAP1 / FURFURAL / HIPPURIC ACID / 686-11-04 CATALCG OF GAS CHRCMATCGRAPHIC RETENTICY DATA F'3R URINARY CONSTITUENTS 4ND RELATED COYPOUNOS/ 68PRR-037 HROMATOGRAPHY/ IDENTIFICATIOY OF URINARY CONSTITUENTS ISOLATED BY AYION EXCqANGE C 6eA-D4-C3A HRCMATOGRAPHYl lOENTIFICATlON OF URINARY CONSTITUENTS ISOLATED 8Y ANION EXCHANGE C 68PRR-010 HRCPATOCRAPHYl IDENTIFICATION OF URINARY CONSTITUENTS ISOLATED BY AYION EXCHPNGE C 68PRR-086 ANIGN EXCHANCE CH91MATOGRAPHY OF HYDRCLYZED URIYE/ 68A-04-038 S OF FRACTIONS FROM TPE ANICN EXCHAYGE CWOMATOGRAPHY OF URINE/ GAS CHROMATOGRAPHIC ANALYSI 6BA-04-03D G OF FRACTIONS FROM TVE ANION EXCHAUGE CHROMATOGRAPHY OF URINE ( MASS SPcCTRCMETRY OF UPlNE COMPONENTS )/ 68A-D4-03E FRACTIONATION OF URINE BY CEL AND ANION EXCHANGE CHROMATOGRAPHY/ 68A-04-03C FRACTIONATION OF HUMAN URINE BY GEL CHRCMATOGRAPHYI 68PRR-084 EXCHANGE CHPOYATOCRAPhY OF URINE ( YASS SPCCTROMETRY OF URINE COMPONFNTS )I DESALTING OF FRACTIONS FROM T 68A-04-03E ROLE OF THE LARGE NATIOYAL RESEARCH LABORATORIES IN THE USA/ THE bRPRR-100 R PREDICTING CRADES IN RELATEE CRAFT TRAINING/ VALIDITY CF SCME TESTS OF INTELLECTUAL ABILITY FO 68PRR-PO5 STUDIES OF VARCUMl 6BA-07-01C 4 ENF 3.17 CICNE I Dl RRCMO FLUOPENE / TRUXENE / UREA I VdRCUM I Pap! I FURFURAL / HIPPURIC ACT@ I CARYOP 688-11-04 PREPAPATIVE GAS CHROMATOGRAPHY ( VARIAN-AEROGRAPH PREPARATIVE GAS CHROMCTOGRAPH I/ 68A-02-01G STLOIES RELATED TO PRGJECT SALT VAULT/ 6eA-C E-C7G BAf AUTOMATIC POTENTIOMETQIC TITRATOR. VELOCITY SERVO, ORNL MODEL-P-1728 AND MODEL-Q-172 h8PRR-078 G FUNDAVENTAL POLAROGPAPVIC DATA/ EVALUATION OF VERTICAL ORIFICE RAPID TEFLON D.M.E. FOR OBTAINUIN 68A-02-086 AROGRAPHY OF URAYIUM IN 1 MOLAR HYDQCFLUORIC ACID WITH 4 VERTICAL ORIFICE TEFLCN DROPPING MERCURY FLECTROO 6eA-DZ-DPR NALYSIS IN TAPERED TRANSITICN JOINTS IN RtACTOR PRESSURE VESSEL/ STRESS A 68TR-01 PORT/ STANDARD REFERENCE YATERIALS AS VIEWED BY THE LABORATORY SUPERVISOR - A STATUS RE 68PQR-034 NSIONALLY ROTATING SAYPLE PCLOER FPQ 14-MILLION ELECTRON VOLT NEUTRON IRRADIATIONS/ THREE DIME 68PRR-012 MOOIFICATIOY OF DUAL SET POINT VOLTAGE CCMPARATOR ( ORNL MODEL-'2-2950 I/ 684-01-15 CONTROLLED POTENTIbL CONTROLLED CURRENT CYCLIC VOLTAMMETER/ 686-01-12 CONTROLLED POTENTIAL AND CONTROLLED CURRENT CYCLIC VOLTAMMETER/ 68PRR-051 WITH THE CONTROLLED POTENTIAL CONTROLLED CURRENT CYCLIC VOLTAMMETER/ DERIVATIVE CIRCUITS FOR USF 688-01-13 CDNTROLLEO POTENTIAL DC PCLAPOGRAPH VOLTAMMETER I YODEL-'3-27921 68PRR-050 RENT/ CYCLIC VOLTPMMETERt CONTRCLLEO POTENTIAL, CONTROLLED CUR 6BPRR-072 A VOLTAMMETRIC METHOD FOR FLUORIDE/ 68PRR-036 ORIDE - BERYLLIUM FLUORIDE - ZIRCONIUM FLUORIDE AT 5DOCI VOLTAMMETRIC STUDIES OF CHROMIUM(I1I IN MOLTEN LI 68PRR-110 ISK ELECTRODE / ROTATING PYROLYTIC GRAPHITE ELECTRODE I/ V3LTAMMETRIC STUDIES OF PLUTONlUMt NEPTUNIUMI AN0 6eA-02-C70 E, REVERSIBLE, OVEPLAPPIYG WAVES IN STATIONARY ELECTRODE VOLTAMMETRY/ ON THE SEPARATION OF HALF-WAVE POTEN 6BA-01-14 €7 REVERSIBLE. OVEPLAPPING WPVES IN STATIONARY ELECTRODE VDLTAMMETRYI ON THE SEPPRATIOY OF HALF-WAVE POTEN 68PRR-025 M FLUORIDE - SODIUM FLUORIDE POTLSSIUM FLUORIDE PELTS CN VOLTAYYETRY AT PYROLYTIC GRAPHITE AND PLATINUM ME 6BA-03-021 THIN FILM MERCURY ELECTRODt VOLTAMMETRY OF BISMUTH/ 6 88- 10- 10 ORlOE - eERYLLlUM FLUORIDE - ZIRCONIUY FLUCRIOE AT 5DOC/ VOLTAMMETRY OF CHRCMIUMIII) IN MOLTEN LITHIUY FLU 68A-03-C2B RAOIONUCLIOES IN HIGH FLUX ISOTOPE REPCTOR COOLPNT WATER/ 6eA-08-06H LINE kbTER / IhTERFERENCES TD hINKLER METHOD / DEAERATE0 WATER / CARBON 01 CXIDE I/ CEAERATION SYSTEMS ( 0 6eA-02-04C OXIDE I/ DEAFPATION SYSTEMS ( DISSOLVED OXYGEN / SALINE WATER / INTERFERENCES TO WINKLER METHOD / OEAERIT 68A-02-04C NICKFLATE(I1 / POTASSIUM NICKEL(1VI PARA PER IODATE 112 WPTER / POTASSIUM TETRA CYANO NICKELATE(1I) / TET 68A-09

A RESIN FOR DESALTING AND REMOVING ORGANIC COMPOUNDS FROM WATER I ACETATE / AMBERLITE XAD-2 I/ EVALUATION 0 68A-02-058 ANALYSIS OF WATER SYSTEMS/ 688-02-04 NALYZER / HYCROPONIC BEDS / ALGAL NUTRIENTS I/ EUTROPHIC WATER SYSTEMS ( PHOSPHATE I NITRATE / TECHNICON A 68A-02-048 QUIRED FOR RESOLUTION OF SIMPLE, REVERSIRLE, OVERLAPPING WAVES IN STATIONARY ELECTRODE VOLTAMMFTRYI ON THE 6BA-01-14 142

QUIRED FOR RESGLUTION OF SIMPLE, REVcQSIBLE7 OVEPLCPPING WAVES IN STATIONARY ELECTPZIOE VOLTAMMETRY/ ON THE 6BPRR-CZ5 0 IN AN ORGANIC SYSTEM/ LIQUID SCINTILLATION CCUNTING OF WEAK BETA EMITTERS IN AQUEOUS SOLUTION BY USE OF 6fiA-08-02G ON X-1001 LIQUID SCINTILLATION COUNTIVG OF WEAK BET4 EMITTERS IFU ABUEOUS SOLUTION USIhC rQIT t8pPR-C45 N TRAVEL TO CZECHOSLOVAKlAt ITALY. ZWITZFRLANO. GERMANY. WEST GERMANY, NORWPYv AVO ENGLAND, SEPT.2-30rlC67 68PRR-047 RY OF SUBSTANCES ISOLATED BY THIN LAYEP CHRCMATOGRAPHY ( WICK-STICKS )I INFRAREO SPFCTROYFT 6PA-02-DZG / MODIFIED WILLARD - WINTER DISTILLATION METHOP FOR FLUOQICE hFP-10-13 APPLICATIONS OF A SERYLLIUM WINOOW GERM4NIUM - LITHIUM SPECTRnVETER SYSTEiI/ 68A-Ce-r)3C SALTS I/ CONTPINEPS FOR MOLTEN FLUORIOF SALTS ( DIAM@ND WINDOWED CELL FOR SPFCTQOPHOTOMET9IC MFASUREMENTS heC-03-02F DROPORTIOMAL BETb COUNTER, WINDOWLESS/ 6PPR Q-070 EMS ( OISSOLVEC OXYGEN / SALINE WATER / INTERFEREVCES TO WINKLER METHOD / OEPERATFO WATER / CARPON 01 C'X13 6PA-D2-C4C MODIFIFD WlLL4RD - WINTER DISTILLATION METHOD FOR FLWQI'JEI tee-1 c-13 X-PAY AN0 OPTICAL SPECTRCCHEMISTRYl 688-05 X-RAY SPECTROSC7PY/ 68A-05-01 G OF WEAK BETA EMITTERS IN AQUEOUS SOLUTION USING TRITON x-1001 LIQUID SCINTILLATION CDUNTIN 6RPFQ-045 WEAK BET4 EMITTERS IN AQUEOUS SOLUTIOF! RY LSE OF TRITON x-in0 IN 4~ ORGANIC SYSTFYI LIQIJID SCINTILLATICN 684-08-G2G OVING ORGANIC CCMPOUNDS CROM WATER ( ACETATE / AMBERLITE XAO-2 I/ EVALUATICN OF A LIPOPHILIC ADSORPTIOV WE 6RA-02-058 THE DECAY CHAIN HAFNIUM-I72 GOES TO LUTETIUM-172 GOES Tc1 YTTERRIUN-172/ INVESTIGATION GF GAYYA-9AYS IN 68PRR-115 / RHODIUM-103M / RUBICIUM-84 / IODINE-129 / IODINE-130 / YTTRIUM-91 / THULIUM-170 )I CHARACTERIZATION OF I 68A-08-fl60 REPORT OF FOREIGN TRAVEL TO CZECHOSLOVAKlAt YUGDSLAVIAr AUSTRIAr GREECF. PUC.29-OCT.8rla67/ 6RPP.R-043 UTONIA / PROTPCTINIUM / TRANSURANIUM ELEMENTS / URANIA / ZIRCONIA )I HIGW LEVEL ALPHA RADIATION LARCRATORY 68@-12-01 UM(IV1 IN MOLTCN LITHIUM FLUORIDE - RERYLLIUM FLUORIDE - ZIPCONIUY FLUORIDE I 65.6-29.4-5.0 YOLE PEPCFiiT I hRPRQ-022 UMIIV) IN MOLTEN LITHIUM FLUORIDE - BEFYLLIUM FLUORIDE - ZIhCDNIUW FLUORIDE PT FAST SCAk RATES AND qHflPT T 6PPFQ-108 IUMlV) IN MOLTEN LITHIUM FLUCRIOF - EERYLLIUM FLOORIOE - ZIRCONIUM FLUOkIDF PT 500C/ CISPROPORTIONATIDN OF ce~-03-024 IUM(V) IN MOLTEN LITHIUM FLLORIOE - BEPYLLIUM FLUOFIDE - ZIRCONIUM FLUOQIOE AT 5ODC/ DISPROPORTIONATION OF 68PRR-DZ3 IUMIVI IN MOLTEN LITHIUM FLliOPlOE - BEQYLLIUM FLUORIDE - ZIRCONIUM FLUORInE PT 500C1 DISPROPCRTION4TlnN OF 6PPRR-109 uncrr) IN MOLTEN LITHIUM FLUCRIDE - PERYLLIUM FLUORIDF - ZIRCONIUM FLUORIOF 4T 500CI VOLTAMMFTPIC STlIPI~S 6PPRR-110 UMIII) IN HOLTFN LITHIUM FLUCRIDE - BEPYLLIUM FLUORIDE - ZIRCONIUM FLUORIDE PT 5DOC/ VOLTPYMETFY OF CHROMI 688-03-028 / POLAROGRAPHY OF ZIRCONIUM IN ACETONITRILE ANI? DI YFTHYL SULFOXIDE 6RA-01-07 URESl OETERMINPTIOY OF H4FNIUM AUD ZIRCONIUM IN HAFNIUM GXIOE - ZIPCCNIUM CXIDE MlXT 688-10-07 ETERMINATION OF HAFNIUM 4NO ZIQCDNIUM IN HPFNIUM OXIDE - ZIRCONIUM OXIDE IMIXTURESI 0 6AP-10-07 PING MERCURY ELECTRODE/ PPPIC POLAROGRAPHY PF UP4NIUM IN 1 POLAR HYORCFLUORIC 4CID WITP A VERTICAL DRIFICE 6SA-OZ-CBB 0 01 NICKFLITEfIl 1 POTASSIUM NICKELIIV) PARA DER IDDATE 112 WATER I POTPSSIUM TETRA CYAN9 NICKELATE(!II / h8A-09 P4RTICLE SIZE DISTRIRUTION OF PARTICLES FROM 10 TO 2OPO MICRChS eY SEDI'IENTPTION ANPLYSIS/ 68PRR-CC7 V NEUTRON-GENERPTDR STUDIES ( DETERMINATION OF OXYGEN BY 14-MEV NEUTRON ACTIV4TIDY I/ 14-ME 6PA-D@-05b DETERMINATION OF FLUORINE IN FLUORSPAR BY 14-YEV NEUTRCN ACTIVATION ANALYSIS/ 68A-08-05B 14-NEV NEUTRON GENERATOQl 686-08-05 OF OXYGEN BY 14-MEV NEUTRCN ACTIV4TION )I 14-HEV NEUTPON GENEPPTOR STUCIES ( OETERMINATITY 6RA-0 e- C5 4 STANDARD GAMYA-RAY SPECTRA OF THE ELEMFNTS FOLLOkING 14-MEV NEUTRON IRRADIATIONS/ 6BPRR-121 14-MEV NEUTRON REACTION RESEARCHI bRA-Oe-05D THRFE DIMENSIONALLY ROTATING SAMPLE HCLDER FOP 14-MILLION ELECTROY VOLT NEUTRON IPRADIATIONSI 68PRR-C12 PECTROSCOPY IN THE NEUTRON DEFICIENT MASS NUMBEF BETWEEN 173-185 REGION/ NUCLFCQ S 686-08-030 ETHYL BENZENE SULFONATF / ESTROLOL4CTDNE / 2 BETA METHYL 19 NOR TESTD LOLACTONE / 2 ALPHA METHYL ESTQA 4 E 6AB-11-04 HE ANALYTICAL CHEMISTRY DIVISION 4NNU4L PROGRESS REPORTS 1964-1967/ CUMUL4TIVE INDEXES TC T 68PQR-056 THLY SUMMARY - NOV.,1967 / DEC.,1967 / JAN.rl968 / FEB., 1968 / MAR.,1068 / APR.11968 1 MAY,1968 / JUNE119 68PRR-CbC ESTROLOLACTONE / 2 BETA METHYL 19 NOR TESTO LOLbCTONE / 2 ALPHA METHYL ESTRA 4 EN€ 3.17 CIONE / 2 BFTA ME 68B-I 1-C4 ESTC LOLACTONE / 2 PLPHA METbYL ESTRA 4 ENE 3,?7 DIONE / 2 BETI METHYL ESTRA 4 ENE 3.17 DIONE / DI BQOMO F 68R-11-04 / BARIUM PARA ETHYL BENZENE SULFONATE / ESTROLOLACTONE / 2 BETA METHYL 10 NOR TESTC LOLPCTDNE / 2 ALPHP ME 688- 11-04 LY TETRA FLUORO ETHYLENE ( TEFLON I AS 4N AOSDRBENT ( 01 2 FTHYL HEXYL CRTHC PHOSPHORIC ACID / HDEHP / LIQ 68A-flZ-CEB ON EXCHANGERS 11 RECLAIMING 4MIND ACIDS - CARRON-14 ( DI 2 ETHYL HEXYL ORTHC PHOSPHDQIC ACID / HOEHP / LIB 68A-04-016 ES I AMFRICIUM / EUROPIUM / HEX4 FLUORU ACETYL PCETONE / 2,216r6 TETRA METHYL 3.5 HEPT4NE DIONE I/ PREPARA 684-02-076 PARTICLE SIZE DISTQIBUTION OF PARTICLES =ROM 10 TO 2000 MICRCNS BY SEDIMENTATION ANALYSIS/ 6QPRR-CO7 ETHYL ESTRA 4 ENE 3,17 DIONE / 2 BETA METHYL ESTPA 4 €NE 3.17 DIONE / 01 PPCMG FLUClRENF / TRUXENF / UREA / 688-11-04 THYL 19 NOR TESTO LOLACTONE / 2 ALPHA METHYL ESTRA 4 ENE 3.17 DIONE / 2 GET4 METHYL ESTRA 4 Ei4F 3.17 OIONE 688-11-04 PlUM I HEXA FLUORO ACETYL ACETONF I 2r216-6 TETRA YETHYL 375 HEPTANE DIONE I/ PREPARPTION AN0 ANALYSIS OF 68A-fl2-07G ACIDS BY LIGAND EXCHANGE CHRCMATOGRAPHYl ASSAY OF 3/ TERMINAL YUCL€OSIOES UF TRANSFER RIP0 NUCLEIC 68PR R- 0 8 5 N MOLTEN FLUORIDE SALTS )I ABSORPTION SPECTRA OF SEVERAL 30 TR4NSITION YET4L ICUS IN MOLTEN FLUORIDE SOLUT bP4-03-D2G LPHA METHYL ESTRA 4 ENE 3717 OIONE / 2 BETA YETHYL ESTRA 4 ENE 3717 OIONE I CI BROMO FLUORENE / TRUXENF / 668- 11-04 ETA METHYL 19 NOR TESTC LOLACTONE / 2 ALPHA METHYL ESTRB 4 ENE 3917 OIONE / 2 BETA YETHYL ESTRA 4 ENE ?,I7 688-11-04 ALCCHDL / FURPN ALCEHYOE I ORGAN0 PHOSPHOQUS POLYMERS / 5 FURFURYL FURFURYL 4LCOHOL / DEUTERO 01 METHYL S 688-11-04 UH FLUORIDE - EERYLLIUM FLUORIDE - ZIRCONIUM FLUORIDE AT SOOCI OISPROPORTIONATION OF ELECTROCHEMICALLY GEN 6RA-03-CZA UH FLUORIDE - eERYLL1UM FLUORIDE - ZIRCONIUM FLUORIDE AT 5DOCI OISPKOPORTION4TION OF ELECTROCHEMICALLY GEN 68PRR-023 UM FLUORIDE - PERYLLIUM FLUORIDE - ZIRCONIUM FLUORIDE AT 5DOC/ DISPROPORTICNATION OF ELECTROCHEMICALLY GFN 6ePRR-109 UM FLUORIDE - BERYLLIUM FLUORIDE - ZIRCONIUY FLUORIDE AT 5OOCI VOLTAMMETRIC STUDIES OF iHRc1MIUM(lI) IN MOL 6bPRR-110 Ut4 F~UORlDE- EERYLLIUM FLUDRIOE - ZIRCONIUM FLUORIDE AT 5DDC1 VDLTAYMETRY OF CHROMIUM(II1 IN MOLTEN LlTHI 681-03-028 ROM IN REPCTOR TESTS OF REACTOR FUEL ELEMENTS I MONOPOLE 600 RESIDU4L G4S ANALYZER I/ ANALYSIS OF OURGE G4 68A-03-03A IUM FLUORIDE - BERYLLIUM FLUORIDE - ZIRCONIUM FLUORIDE ( 65.6-29.4-5.0 VOLE PERCENT I EVIDENCE FOR ADSORPT 6PPRR-C22 RCK SILlC4 GEL G / MASS SPECTRUM OF CORNING POROUS GLASS 7935 / MASS SPECTRUM OF GEL'4AN ITLC-SA YEPIUM / M 684-02-02F Author Index

A

APP1.E. Q. F. hRA-01-0 1A APPLr. R. F. 6Q4-03-018 APPI F. R. F. 6PA-C3-01C 4"PLE. 9. F. h8D-14-C5R APPLE. R. F. 68PRR-091 PPP1.E. R. F. hRPRR-097 6eR-12-fl5

ATT2ILL. J. E. 68A-04-03H bRA-('4-011 ATTRILL, J. E. 688-04-031 hf3A-C?4-n3A ATTRILI. J. E. hRA-04-04 hdA--P4-Q3R OQA--04-"3C hRPRR-CO9 B 0 RPQR--0 10 h8PRR-006 4 PP RR-nR4 hAPRR-nSS 68PRR-786 69PRR-CCh

6qA-04-030 BATE! L. C- h8A-08-0 1E 694-P 4-03F RATE. L. C. 684-08-040 h3PRR-037 R4TFt L. C. 68A-nR-04E RATE. L. C. h 8A-0 9-04F C P.ATF. L. C. bP4-08-059 HPTE. L. C. 6XPRR-nOZ CAPFRON. A. E. hRA-cb RATF. L. C. 6XPRR-007 TAMERON, 4. F. 4PY-11 RATF. L. C. 68PRR-011 CAb'ER@N. 4. E. 68E BATF. L. C. 69PQQ-Pl2 CAYFROY. 4. E. 68PRR-127 - 128

68A-08-06F CANADA. 0. C. 685-1 0-94 6RPRQ-017 Cbk'AD4. D. C. h~-io-n5 CANADA. C. C. 6x3-10-06 CANAll4. 0. C. bRB-1 C-0 7 RFLFW. H. L. 68A-01-05 tAN4DA. r). C. hSR-lO-n8 RELFW. W. L. 684-01-06 CANADA. C. C. 6EPRR-OR7 BFLEW. W. L. 6RA-0 1-07 RECFW. W. L. 68A-01-09 RFLEM. W. L. hRA-0 1- 11 CAQTEQ. J. A. 69A-06-0 1 9FLFW. W. L. 6 R A-0 1-2 2 CIRTFR. J. 4. 6RR-11-02 RCLFW. W. L. 68A-C! 1-2 3 RFCEH. W. L. 6RE RFLEU. W. L. b8PRR-083 CATON. J. E. 6RA-03-01 B

68PHR-308 CclRISTIE. W. H. bPA-06-r?4

=RELL. P. R. 68A-08-02H ~RA-Q~-~ZO 6R4-08-92F 68H-10-02 68PRR-115 h P B-12-0 1 h8PRR-01 3

=RIGGERS. R. E. 68PRR-008 COOPER. A M. 0. 68PRR-034 =BIRD. F. 0. 68A-08-01F

6RR-10 686-12 68A-08-04C 68E

143 144

CnSTANZO. 0. A. h8B- 10- 12 FFLOMAN. C. 68A-05 COSTANZOI D. A. 688-1 0-1 3 FFtflMAN. C. 68A-0 5-0 2 FELDMAN. C. 68A-O 5-03 FELDYAN. C. h8A-0 5-04 =GRIST. L. J. 68A-02-02E FEIDMAN. C. 6 8 A-0 5-05 =GRIST. L- J. 6 8A-0 2-02F FFLDMAN. t. 6RE =tRIST. L. J. 6 fl A-0 2-0 2G FELOMAN. C. 6RPRR-OR9 =GRIST. L. J. h80-14-05A =GRIST. L. J. 68PRR-076 h9A-0 5-04

ICIINEll. D. R. 68A-08-04R =FISCHRACH. H. 68PRR-034 D

DALE. J. M. 68A-03 FISHFR. 0. J. 68A-01 DALE, J. Ma 68A-03-0lA FISHEF. n. J. 6 8 A-0 1-0 2 DALE. J. M. 69~-n3-0in FJSHFR. D. J. 6 RA-0 1-04 DALE. J. M. bE1A-03-0ZR FISHFR. 0. J. 6RA-01-05 DALE. J. H. 68E FISHFP. 9. J. 6 R A-C 1-06 DALE. J. N. 6RPRR-OR 7 FISHER. 0. J. 6AA-01-08 0AI.E. J. M. 4 8PRR- 11Cl FISHFR. 0. J. 6RA-nl-09 FISHFR. D. J. 684-0 1- 1R FIWFR, n. J. 6 84-0 1-2 1 6RD- 14-0 2 FISHFR. 0. J. 688-01-23 FISHER. 0. J. 6 SD- 14-02 FISHFP. fJ. J. hRD-14-05A 6RPRR-057 FISHW. 0. J. 68E h8PRR-OR8 FISHER. 0. J. 68PRR-033 FISHFR. D. J. 6 RPRR-04 e FTSHFR. ID. J. 6 8PRR-0 97 =DEAN. J. A. 6RA-C'2-0 1H =DFA"I. J. h. 6RD- 14-0 1 =DFAY. J. A. b 8 D- 14- 04 :FLnRENCF, T. M. hPA-Ol-C? =OFAN. J. A. 68PRR-OR3 -FIflRENCFt 1. M. h8A-01-11 zFIflRFNrF, T. V. 6RPRR-036

6RA-05-0 1 h RD- 14-0 7 G 6 8 4-0 8-12 4 R AQPRR-046 I)YFR. F. F. 59A-08-04C OYER. F. F. ARA-28-04D DYFR. F. F. h8A-CP-n4E AR8- 1O- 14 OYFU. F. F. h 8A-@R-O4F DYFR. F. F. h R A-08-Q 5 8 DYFQ, F. F. 6HPRR-fl02 nYER. F. F. bPPRR-007 DYCR, F. F. 5RPRR-C11 DYFQ. F. F. h8PRR-nl2

E

rqy. R. F. 6RB-11-OlA

ELP'D.IDGE. J. S. 64A-f9-Q2H EL0Q.IDGE. J. S. 5 QA-CR-03A FLORIDGF. J. S. 5RA-OR-C6F hRA-C 2-nlA El 09106E. .I. 5. h8A-08-0hG hRA-OZ-OlC FLDRIDGE. J. S. ARE ARA-02-Cl0 FLnPInGE. J. s. 6ADRQ-017 6~a-r2-n 1ti hRA-02-13A 644-"7-04A €ldc'D.Y. J. F. b8A-n 8-n 1F h R A-0 2 - 1' 5 A FMFPYI J. F. hRA-CR-22F 6 9 442-"5c E"FPY. J. F. 684-Cq-93R ARA-"7-nh EMFPY. J. F. 68A-OR-? 3C hm- 14-04 FYEQY. J. F. 4 R A-n4-'13 F EHFQY. J. F. h4A-08-04A FMFQY. J. F. 69A-C8-060 q A- o 7 - 4 rf FIJEPY. J. F. AAA-P8-QAE 6 A-i' 2 -D 7 D EMFQYt J. F. 630-14-05A 6QA-"?-C7 I EMFQY. J. F. 68PRK-Q?9 580-1 4-92 FMFDY. J. F. h AQRK-057 SRP9R-033 EMFQY. J. F. AHPK9-f 94 H :HAliN. P. L. hRPRR-Pl4 F HAF'iJ. K. I-. hPPRR-Pl5 FARRAP. L. G. 'HAH1.I. P. L. At.'PQK-P7" FARRAP.. C. G. :HAW. P. L. ARPPR-115 145

PPKL)LFY. T. E. hRA-CS--:lA KFLL.FY. 1J. T. HAYllLrY. T. IH. 68A-PR-71C KFLLCY? 4. 1. +JhNOLFY1 T. H. 5 R A-C: 9 -0 2 0 KTLLFY. Y. T. H3NI)lFY. T. W. 6RA-nU-?ZE KELL~YI Y. T. IihhOlFY. 1. H. bR4-0q-73D KFLLFY. Y. T. IIANPLFY. T. H. haA-C8-n4a KFLLFY. q. T. H\lili)lfY. T. H. h 8 P R R - ”46 KFLI.EY. 1J. T. H4Y17tFYq T. H. 4RPRR-113 KFLLFY. ‘4. T. HA‘JDL~Y. T. H. hHPicR-115 KCLI.FY. 4. T. KFLLFY. M. T. KFLLFY. ”. T. KFLLFY. M. T. KFLLEY. ”. T. KFLLEY. M. T. HAPMIIN. T. G. KFLLEY. Y. T. KFIIFY. H. T. KFI-LFY. M. T. 4R 4-P4’-i? 18 KFLLEY. r4. T. hd4-04-01F KTLLEY. M. T. 684-(\4-71C, h 8 A-O4-,2 1H =KT*. Y. K. hRD-14-96

HFPTFL. C,. P. hKA-?h-”3 IiF‘QTFL. G. R. bPA-“6-‘3?H IH‘9TEL. t. K. 6RPRQ-016

=KqPIIS. F. F. fx R A-(; 7-02C =HILSF. K. M. 6YA-04-331 =KQALJS. F. F. UHPRR-027

Hr’l SPPPLE. H. L. 688-13-1 1 KllilflTA. P. hRA-C A-779 Kll?flTA. H. hYA-”8-07C K!IR?TA. H. b 8 4-1- u - 7 D Hfl!,TON. 4. 0. h 8 A- 0 7 -27 1 H KVRQTA. H. 684-@8-Q7G HCKTDN. A. 0. 6PA-@2-?1C KiJDilTh. H. 68PRP-Pl8 H(:KTO?:. 4. D. 684-nZ-filF KIJHUTA. H. 4 9PPK-019 HIlCT9hl. 4. 0. h94-D2-”1F K119’1T4. H. hPPrlK- 173 HORTUN. 4. D. hEA-r?Z-nlG K!lR:lT4, H. 6RTQ-01 HO‘ITON. 4. D. 6 RD-14-05 8 KIJPCITA. H. 6 3T K- C 2 H:lRTflY. 4. 0. 4pF 1 HflPTilN. C. A. 6RE

IIHIIPF. H. 8. 684-0 8-06 F =LAITINEN. H. 4. 0170-1 4-01 OHIIPF. H. W. 6RPRR-017

J 6 R 8- 12-93 685 =JFNKIN<. H. W. 6 H 4-03-9 2C =JCI\KIN<. H. W. 6UD-l4-”74 h HPRX- 059

JCNFS. F. S. h 84-0 5-0 3 LAVALI F. 0. E. h8A-09

JOWF5. H. C. 6RA-01-01 JClNFC. H. C. 684-0 1-02 :LFPRI. ‘4. A. 6UA-P 8-(?7E J‘INFC. H. C. 6RA-01-09 :LfPRI. M. A. SRA-OR-03F J‘INFS, H. C. hYA-01-12 :LFPRI. H. 4. 4PD-14-1)5A JOKFC. H. C. 684-01-15 JI)NEC. H. C. bA4-01-16 JINFS. H. C. bRA-C 1-1 7 :LODYELL. J. 0. 684-02-01G JINES. H. C. 68A-0 1- 1S :LOllh(ELL. J. 0. 680-14-05R JONFC. H. C. h8A-01-22 J‘INES. H. C. h AI\-0 1-2 3 Jl3NFS. I-(. C. 69PRR- 048 LllhtCl. J. R. JONFC. H. C. hRPRR-077 LIIQD. J. R.

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6RD-14-04 YIIIUNG. J. P. h R A-n 3- 97 0 YPIING. J. P. 6RA-r)3-C2E YflllNG. J. P. h 8 A- 0 3 - (1 2 F =TIITHILL. 5. M. h A P RR- 0 3 L Yf'llNG. J. P. h 8 A-? 3 -P 2 G YPIJYG, J. P. A-0 V 68 3-Q 2 14 YPUNGv J. P. 54A-C3-n21 =VIGO. 5. 6APRR-1134 Y'7UNG. J. D. 6AD-14-fl4 Y'lllYG, J. P. f> 8 D RR- Cc) 6 Y'?IJNG. J. P. 6PPRP-12 7 w YPUNG. J. P. 6HPRR-124 WAGNFU. E. R. h P P R R- 0 7 8 Z

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A NA LY T IC A L CH EM IST RY DI V ISION

NOVEMBER 1, 1968

I I ADVISORY COHMlTTEE I STAFF CONSULTANTS M. L. MOSS, EXP 12-31-71, INSTITUTE FOR MUSCLE H. R BEATTY.' BUDGETS AND COSTS A L. HARROD. ADMlN ASST. J A DEAN, UNIVERSITY OF TENNESSEE DISEASE. INC, NEW IORK. N Y C L BURROS.' RADIATION AND SAFETY OFFICER D B WAGOYER GLEB MAMANTOV, UNIVERSITY OF TENNESSEE G H MORRISON, EXP 12 31 69. CORNELL UNIVERSITY J S ELDRIDGE.' COORDINATOR FOR RADIOCHEMICAL JEWELLNORMAL R FRAKER,SECRETARYELLIS. SECREi:.?Y A 0. C. NIER. UNIVERSITY OF MINNESOTA H A LAITINEN EXP 12-31-70 U*IIYFR

I ANALYTICAL SERVICES I RESEARCH ANDDEVELOPMENT MASS AND ELllSSlON L 1.CORBIN. ASSISTANT DIRECTOR SPECTROULTRY 1Y.12) JEAN C POPE.' SECRETARY A E. CWERON. ASSISTANT DIRECTOR LINDA F AMBURN. SECRETARY I I L DORISC WITH. SECRETARY

HIGH.LEVEL RAOIATION FACILITY &RAY AND SPECTROCHEMISTRY ANALYTICAL INSTRUYENTATION I I NUCLEAR AND RADIOCHEMISTRY C.L. BURROS' AND EVALUATION LABORATORY I I C. FELDMAN. SUPERVISOR 0 1. FISHER. GROUP LEADER W. S LYON. JR ,GROUP LEADER J. R. SITES, SUPERVISOR P. F. THOMASON. GROUP LEADER H.ZELL W. DUNN COMBS' WR L W STELZNER.BELEW ASSISTANT GROUP LEADER LH. H.C ROSS.BATE ASSISTANT GROUP LEADEN E. J. SPITZER, ASST. SUPERVISOR D c. CANADA' .*.L"ITI D A CDSTANZO N. MARION FERGUSON W L MADODX F. F. DYER G. GOLDBERG F.S JONES I. R. MUELLER J 8. ELDRIOGE' R. C. BRYANT HF. L. HOLSOPPLEMOORE W. R. MUSICK J. F EMERY L. GUINN C A. PRITCHARD 1 H HANDLEY MABEL M. HONAKER INALllT R. L. SHERMAN 8. 0. LUPICA W. E BAYLESS ANNAM YOAKUM S A REYKXM' .W.L",TI E RlCCl A. H. MARSHALL 1. E. STRAIN KATHERINE K. MrDANIEL H KUBOTA TRANSURANIUM MASS SPECTROMETlll E ONKST H E ZITTEL GENERAL HOl.ANALISES LABORATORY HIGH.LEVEL ALPHA RADIATION LABORATORY ROBERTAM RWSEI R E EBY SUPERVISOR.*.LIST, C. E. LbMB. SUPERVISOR J n COOPER. SUPERVISOR Y K KIM'> C. K. TALBDTT. ASST. SUPERVISOR W. F VAUGHAN F. I(. HEACKER I B"ILD,YC 1111 U KDSKELA INILIIT, REACTOR PROJECTS F L. LAYTON .*.L"IT, A. S MEYER. GROUP LEADER ANALYTICAL BlOCHEYlSTRY J. S WIKE G ILGAULT G. R ARCHER W. W. JOHNSON I OPTICAL AND ELECTRON MICROSCOPY -1 J M DALE. ASSISTANT GROUP LEADER W. F. ROGERS K R BOWMAN 0. D. PAIR 1 E WILLMARTH. SUPERVISOR R. F. APPLE GJ GOLDSTEIN.E. ATTRILL GROUP LEADER SARAH W HOPKINS 1 C M BOYD SPECTROCHEMISTRY EVELYN L. VILES T. G. HARMON H. W. WRIGHT J E CATON. JR C A BURTIS. JR 1 WlFT B I*IFT c I*lli IIYlFl BUlLDlHC 700 J A. CARTER. SUPERVISOR I A D HORTON w C.0UTTS .**L"ITI S A MoclNTYRE 1 C. PRICE' S R DINWORE' E. C FEARNOW' R. E JONES' N. C. MEYER, ASS1 SUPERVISOR D L MANNING D W HATCHER c. c FOUST..' **.L"li MARY P HUNTWAN I 0 RUBIN IYALIII L. G FARRAR WANDA C MASSEY I J P YOUNG A L TRAVAGLIN E H WATERS .N.L"IT .*.LIST .*.L"*I .*.L"%T J. M. PEELE LH. wP TURNER"JENKINS~ i W H AKERS A H MATTHEWS R A. JONES 0 E. GiLL A IR1FT B IHlFT c I",*T 0 IHlFT I SCOTT' P W. PAIR' C P BAKER' J D PENDLETDN' 'SHIFT SUPERVISOR G F L WHITING" INORGANIC PREPARATIONS "RELIEF SHIFT SUPERVISOR C. C FOUST'" MASS SPEtTROMETRY RESEARCH 0 E. LmVALLE. SUPERVISOR METHOWLOGY G R HERTEL' ANALIS, A"AL"17 ANALIIT *HILIST R. 0 OUINCY. JR. I W 0 SHULTS. GROUP LEkDER D H SMITH R S NABORS C. COOK. JR J. L. PARRETT H. L. TUCKER M R GUERIN C A HORTON 'SHIFT SUPERVISOR W. R LAING. SUPERVISOR "RELIEF SHIFT SUPERVISOR W J ROSS REFEREE ANALYSIS L J. BRADY, ASST SUPERVISOR J R SIOXELI SERVICE J. L. BOTTS M. V. CONNELLY R L WALKER, SUPERWSOR H. G DAVIS I .*.L"ITI J. A EALY RAOlOlfDTOPES-RA0IDCHE"lSTRY E G MILLER K. W GENTRY LABORATORY J L SHARP C F HARRISON' I E I WYATT. SUPERVISOR H c SMITH E. C LYNN DORA I WHALEY G R WILSON R R RICKARD. ASS1 SUPERVISOR D R. MATTHEWS N WILSON lUIL"IT5 J.J HE MONEYHUNMORION DEVELOPMENT C. SUE ALLEY W T. MULLINS A E CAMERON.' GROUP LEADER EDNA E. BONIFACIUS H A PARKER W H CHRISTIE GERTRUDE8 BROWN M E PRUIlT PERMANENI STAFF MONTHLY WEElLY TOTAL H S McKOWN MARTHA R CHILDS C D STRINGER 'DUAL CAPACITY C A CLARK ADMINISTRATIVE AND CLERICAL 4 9 13 'ON LOAN TO REACTOR CHEMISTRY DIVISION W 1 RAINEY. JR C. J COLEY SCIENTISTS 113 113 ION LOAN TO METALS AND CERAMICS DIVISION J R WALTON .**L"ITI PAULINE S GOODWIN ANALYSTS --_7s 7s 'ON LOAN TO SOLID STATE DIVISION P S GOUGE NORA W. COOK SU0TOI*L 117 &I 201 'ON LOAN TO CHEMICAL TECHNOLOGY OlVlSlON J H HACKNEY J H. DAVIDSON OTHERS *ON LOAN TO ISOTOPES DIVISION G. HICKEY' C. L GHANN 'ON LEAVE OF ABSENCE J 0. HILL I L R HALL ORAU GRADUATE FELLOW I I 'ON'OR& LOANGRADUATE FROM BUDGETDEPARTMENT FELLOW K C. LANNOM R W HARVEY VISITING UT PROFESSOR I I INFRARED AN0 N M. R ROSA L. LEWIS E. C HENDREN' ''STUDENT GUEST (UT) J R LUND GERALDINE OLERICH RUT"K. J NORTHCUTTHOLLAND "VlSiTlNG PROFESSOR [UT1 M M MURRAY B PHILPOT "ALIEN GUEST IIAEA FELLOW) G W ROBINSON i H OXENDINE PATRICIA M ROWAN FLORA B PHILLIPS SUE H. PRESTWOOD , W M SWARTOUT WlLLiE 0 TOWNS J. SLESSINGER, JR KATHLEEN I WEBB N A TEASLEY JR J. T WHITE R. J UNDERWOOD3 c. M WILSON~ W. R. WARREN J. V WINCHESTER

151

ORNL-4343 UC-4 - Chemistry

INTERNAL DISTRIBUTION

1. C. E. Larson 55. M. E. Ramsey 2. A. M. Weinberg 56. J. H. Rowan (Y-12) 3. R. F. Hibbs (Y-12) 57. M. W. Rosenthal 4. H. G. MacPherson 58. A.F.Rupp 5. G.Young 59. H. E. Seagren 6. N. G. Anderson 60. M. J. Skinner 7. J. C. Barton (K-25) 6 1. A. H. Snell 8. S. E. Beall 62. E. G. Struxness 9. M. Bender 63. D. A. Sundberg 10. D. S. Billington 64. E. H. Taylor 11. R. E. Blanco 65. P. R. Vanstrum 12. E. G. Bohlmann 66. G. M. Watson 13. C. J. Borkowski 67. C. W. Weber (K-25) 14-23. G. E. Boyd 68. M. E. Whatley 24. R. B. Briggs 69. G. C. Williams 25. 0. W. Briscoe (Y-12) 70. R. G. Wymer 26. R. E. Brooksbank 71. C. L. Burros 27. K. B. Brown 72. A. E. Cameron 28. F. R. Bruce 73. W. H. Christie 29. S. F. Carson H. S. McKown 30. J. A. Cox W. T. Rainey, Jr. 31. F. L. Culler D. H. Smith 32. J. E. Cunningham J. R.Walton 33. D. E. Ferguson J. R.Lund 34. J. L. Fowler M. M. Murray 35. J. H Frye, Jr. 74. J. H. Cooper 36. J. H. Gillette 75. H. C. Meyer 37. W. R. Grimes L. G. Farrar 38. A. S. Householder F. L. Layton 39. W. H. Jordan J. M. Peele 40. 0. L. Keller C. P. Baker 41. M. T. Kelley C. C. Foust 42. R. F. Kimball P. W. Pair 43. Ann S. Klein J. D. Pendleton 44. T. A. Lincoln T. G. Scott 45. J. L. Liverman 76. L. T. Corbin 46. R. S. Livingston 77. C. Feldman 47. R. N. Lyon H. W. Dunn 48. F. C. Maienschein N. M. Ferguson 49. H. F. McDuffie F. S. Jones 50. K. Z. Morgan W. R. Musick 5 1. Lewis Nelson C. A. Pritchard 52. G. D. Novelli R. L. Sherman 53-54. R. B. Parker A. M. Yoakum 152

78. D. J. Fisher 89. J. M. Dale 79. R. W. Stelzner R. F. Apple W. L. Belew C. M. Boyd H. C. Jones J. E. Caton W. L. Maddox A. D. Horton T. R. Mueller D. L. Manning 80. G. Goldstein J. P. Young J. E. Attrill 90. H. P. Raaen C. A. Burtis, Jr. 91. W. D. Shults W. C. Butts M. R. Guerin D. W. Hatcher C. A. Horton I. B. Rubin W. J. Ross A. L. Travaglini J. R. Stokely 81. W. R. Laing 92. J. R. Sites 82. L. J. Brady E. J. Spitzer J. L. Botts R. E. Eby M. V. Connelly J. A. Carter H. G.Davis S. A. MacIntyre J. A. Ealy R. L. Walker K. W. Gentry 93. P. F. Thomason C. F. Harrison D. A. Costanzo E. C. Lynn G. Goldberg G. V. Pierce H. L. Holsopple W. F. Vaughan F. L. Moore G. R. Wilson 94-97. J. C. White 83. C.E. Lamb 98. T. E. Willmarth 84. C. K. Talbott T. G. Harmon F. K. Heacker H. W. Wright U. Koskela 99. E. I. Wyatt J. S. Wike 100. R. R. Rickard S. R. Dinsmore D. R. Matthews E. C. Fearnow J. H. Moneyhun R. E. Jones J. E. Morton J. C. Price W. T. Mullins 85. D. E. LaValle H. A. Parker R. B. Quincy, Jr. M. E. Pruitt 86. W.S. Lyon C. D. Stringer 87. H.H. Ross 101. H. A. Laitinen (advisory committee) L. C. Bate 102. G. H. Morrison (advisory committee) F. F. Dyer 103. M. L. Moss (advisory committee) J. S. Eldridge 104. L. B. Rogers (advisory committee) J. F. Emery 105. J. A. Dean (consultant) T. H. Handley 106. G. Mamantov (consultant) S. B. Lupica 107. A. 0. C. Nier (consultant) S. A. Reynolds 108. Biology Library E. Ricci 109-111. Central Research Library J. E. Strain 1 12. Laboratory Shift Supervisor H. Kubota 113-114. ORNL - Y-12 Technical Library H. E. Zittel Document Reference Section 88. A. S. Meyer 1 15-150. Laboratory Records Department 151. Laboratory Records, ORNL R. C. 153

EX TER NA L DISTRIBUTION

152. Sterling Forest Laboratory, Union Carbide Corporation, New York. 153. J. A. Swartout, 270 Park Avenue, New York 17, New York. 154. R. C. Shank, Idaho Falls 155. T. W. McIntosh, Division of Reactor Development and Technology, U. S. Atomic Energy Commission, Washington, D. C. 20545. 156. duF’ont Company, Wilmington 157. Bettis Plant, Westinghouse Atomic Power Laboratory. 158. William Mott, Division of Isotope Development, AEC, Washington, D.C. 159. Lt. J. C. Courtney, MCL-NI, 1155 Technical Operations Squadron, McClellan Air Force Base, Cal. 95652. 160. Library, Nuclear Fuel Services, Inc., Erwin, Tenn. 37650. 161. J. Frazer, Lawrence Radiation Laboratory, Livermore, Cal. 162. W. W. Grigorieff, Assistant to the Executive Director, Oak Ridge Associated Universities. 163. Research Center Library, Union Carbide Corporation, P.O. Box 324, Tuxedo, New York. 164. Laboratory and University Division, AEC, ORO. 165. W. W. Meinke, Analytical Chemistry Division, National Bureau of Standards, Washington, D.C. 20234. 166-375. Given distribution as shown in TID-4500 under Chemistry category (25 - CFSTI).