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Center for Analytical Chemistry sLjA . ^5 0 NBSIR 81-2425 c^; Annual Report 1981 Center for Analytical Chemistry U.S. DEPARTMENT OF COMMERCE National Bureau of Standards National Measurement Laboratory Washington, DC 20234 October 1 980 Final ssued December 1981 Prepared for U.S. DEPARTMENT OF COMMERCE National Bureau of Standards Washington, DC 20234 NBSIR 81-2425 ANNUAL REPORT 1981 CENTER FOR ANALYTICAL CHEMISTRY C. W. Reimann, R. A. Velapoldi, and J. K. Taylor, Editors U.S. DEPARTMENT OF COMMERCE National Bureau of Standards National Measurement Laboratory Washington, DC 20234 October 1 980 Final Issued December 1981 Prepared for U.S. DEPARTMENT OF COMMERCE National Bureau of Standards Washington, DC 20234 U.S. DEPARTMENT OF COMMERCE, Malcolm Baldrige, Secretary NATIONAL BUREAU OF STANDARDS. Ernest Ambler, Director Certain commercial equipment } instruments } or materials are identified in this report to specify adequately the experimental procedure. Such identification does not imply recommendation or endorsement by the National Bureau of Standards 3 nor does it imply that the materials or equipment identified are necessarily the best available for the purpose. TABLE OF CONTENTS Page I. CENTER FOR ANALYTICAL CHEMISTRY A. Center Overview 1 B. Voluntary Standardization and Quality Assurance 5 C. Pilot National Environmental Specimen Bank Program 9 D. Service Analysis 16 E. Instrument Development Group 18 1. Group Overview 18 2. Selected Technical Accomplishments 19 a. High Reproducibility Analysis with the Infrared Diode Laser 19 b. LEI Ion Collection Dynamics 23 c. Stepwise Excitation Laser Enhanced Ionization Spectrometry 25 d. Spatially- and Temporally-Resolved Studies of Laser-Perturbed Atom Populations in an Analytical Flame 29 e. The Use of Microcomputers in the Center for Analytical Chemistry 33 f. Inorganic Ion-Doped Glass Beads as Potential Microspectrofluorimetric Standards 34 3. Outputs and Interactions 37 II. INORGANIC ANALYTICAL RESEARCH DIVISION A. Division Overview 41 B. Selected Technical Accomplishments 51 1. Application of Sampling Theory to Particulate Biological Samples 51 2. Determination of Ultratrace Platinum in Biological Materials 53 3. A New Method for the Determination of Sulfur by Thermal Ionization Mass Spectrometry 54 4. An Investigation of Biases in the Determination of Sulfur in Steel by Emission Spectrometry 56 5. Determination of Chlorine and Sulfur in Cadmium Sulfide 58 6. Determination of 1-129 in Biological Matrices 59 7. Analysis of Human Liver for Baseline Lead and Thallium 60 8. Development of a Radiochemical Separation Procedure for Tin 62 9. Development of a Fluorescent Glass Standard for Calibration of Instrumentation Used for the Evaluation of Dye Penetrants 63 10. Determination of Halogens in Organic Liquids by Neutron Activation Analysis 64 11. The Determination of Trace Elements in Biologicals and Injectables 66 i Page 12. Application and Evaluation of High Sensitivity Mass Spectrometry for Isotopic and Elemental Abundance Measurements of Uranium and Plutonium 67 13. Development of Improved Matrix Modifiers for Use in Atomic Absorption Spectrometry 70 14. Development of Silica-Gel Procedures for the Analysis of Trace Quantities of Copper and Nickel 72 15. Research to Develop High Accuracy Coulometric Assay Methods for Uranium Metal and Uranium Oxides 73 16. Development of a High Precision Method for the Assay of Milligram Samples of Uranium 74 17. Research to Develop ID/MS for Trace Concentrations of Vanadium 75 18. Investigation of Ionic Chromium Speciation 77 19. Transfer and Analysis of Inductively Coupled Plasma (ICP) Emission Data Using a Mini- and a Main-Frame Computer on the NBS Data Network 78 20. Evaluation of Sources of Error in D.C. Plasma Spectrometry 79 21. Research to Develop Acid Rain Reference Materials. ... 81 22. Design and Implementation of a Solid State Filament Control for Thermal Ionization Mass Spectrometers. ... 82 23. Digital Control Modification for the Varian FR-41 Gaussmeter/Control ler 83 24. Evaluation of a Collimated Ion Collector for Thermal Ionization Mass Spectrometry 83 25. Standard Reference Materials 86 C. Outputs and Interactions 90 III. ORGANIC ANALYTICAL RESEARCH DIVISION A. Division Overview 101 B. Selected Technical Accomplishments 114 1. Relationships Between Liquid/Liquid Partitioning and Retention in Reversed-Phase Liquid Chromatography. ... 114 2. Development of an On-Line Multidimensional HPLC System for Quantitative Analysis of Individual Constituents in Complex Samples 116 3. Methods for the Determinaton of Selected Polycyclic Aromatic Hydrocarbons and Aza-arenes on an Urban Air Particulate Sample and SRM Certification of the Sample 120 4. Methods for the Analysis of Polynuclear Aromatic Hydrocarbons (PAH), Amino-PAH, and Phenols in Alternate Fuels and Effluents 122 5. Methodology for Certification of a Polychlorinated Biphenyl (PCB) in Oil SRM 125 6. Identification of Polychlorinated Biphenyl (PCB) Isomers Using Combined Gas Chromatography/Fourier Transform Infrared (GC/FT-IR) Spectrometry 128 7. Chemically Modified Electrode Detector for Halogenated Hydrocarbons 130 ii Page 8. Electrochemical Oxidation of Croconate Salts and Their Implication in Semiconductor Behavior and Electrochromic Displays 133 9. A Multipurpose Cell for Nonaqueous Electrochemistry. 136 10. Chronoamperometry at Unshielded and Collarless Disk Electrodes 140 11. Spectroelectrochemical Research: Surface-Enhanced Raman Spectroscopy of Pyridine Derivatives 144 12. Measurements of the Optical Rotatory Dispersion of Internationally Exchanged Quartz Control Plates and Long Quartz Rotators Between 400 and 650 nm 145 13. Nitrogen-15 NMR Spectroscopy of Neomycin B at High Field 147 14. Nitrogen-15 NMR and Mass Spectral Characterization of Doubly 15 N-Labeled 2-Amino Oxazoline Derivatives of the Pentoses and Hexoses 152 15. Two-Dimensional Proton NMR Spectroscopy of Hydroxyl Proton Coupled a- and e-Q-Gl ucopyranose 155 16. Comparison of Two Isotope Dilution Definitive Methods for the Determination of Glucose in Serum and Evaluation of the American Association for Clinical Chemistry Candidate Reference Method for Glucose .... 160 17. Comparison of Two Isotope Dilution/Mass Spectrometry (ID/MS) Methods for the Determination of Total Serum Cholesterol 162 18. Identification of Components Leached from Implants Made of Siloxane Polymers and Influence on Prolyl Hydroxylase Activity 163 19. Combined LC/MS Techniques: Development of an Interface System Compatible with Reversed-Phase LC . 164 20. Laser Induced Photodissociation of Ions 166 21. A Method for the Mass Calibration of Photoplates in Field Desorption Mass Spectrometry and Its Application to Some Peptides 170 22. Design of a Toxic Chemicals and Carcinogens Handling Laboratory 173 C. Outputs and Interactions 175 IV. GAS AND PARTICULATE SCIENCE DIVISION A. Division Overview 187 B. Selected Technical Accomplishments 196 1. Development of a Monte Carlo Electron Trajectory Simulation 196 2. Empirical Quantitation in Raman Microprobe Analysis. 198 3. Automation of the NBS Laser-Raman Microprobe 201 4. Development of Standards for Single Particle Analysis of Fly Ash 202 5. Development of a Candidate Thin Film Standard Reference Material 205 Page 6. Intercomparison of NRLXRF Semi-Empirical and NBS Interelement Correction Methods 207 7. Measurement of the Temperature Dependence of the Ozone Absorption Cross-Sections in the Ultraviolet 211 8. Measurement of Infrared Intensities of Atmospheric Species 215 9. Continuation of the Intercomparison of 0 3 , NO, and N0 2 Measurement Standards by Gas Phase Titration 219 10. Studies of the Photochemistry of Trace Airstream Impurities in Ozone Generators 221 11. Determination of Trace Gas Concentration by Infrared Tunable Diode Laser and Fourier Transform Infrared Spectroscopic Techniques . 224 12. Development of Ambient Nitrous Oxide and Halocarbon Standards 227 13. Standards for Measuring Toxic Organic Vapors in the Workplace Atmosphere 229 14. Nitrogen Dioxide Standard for Stationary Source Emission Measurements 231 15. Intercomparison of Aitken and Cloud Condensation Nuclei Counters 233 16. Nuclear Environmental Analytical Chemistry 236 17. Development and Evaluation of Personal Particulate Dosimeters 238 C. Outputs and Interactions 243 I. Center for Analytical Chemistry Curt W. Reimann, Director Ranee A. Velapoldi, Deputy Director A. Center Overview The Center for Analytical Chemistry develops and maintains the scientific competences and the experimental facilities necessary to provide the Nation with the basis for uniform measurements through development of measurement methodology and provision of measurement services in the field of analytical chemistry.' Analytical measurements provide a foundation for scientific and technological research and development concerning materials and their practical application. Moreover, analytical measurements are increasingly used as the basis for industrial, regulatory, and medica 1 decisions. The Center serves as the National reference laboratory for assuring the reliability of analytical measurements. The principal means by which the Center serves as a National reference laboratory is through the development and issuance of standard reference materials (SRM's). The ubiquity of and demand for analytical measurements in modern society is reflected in the diversity of SRM's produced in the Center. These standards are widely used in such diverse areas as the metal and chemi- cal industries and in clinical and environmental laboratories. Each standard is supported by research
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