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Annual Report 1982: Center for Analytical Chemistry AlllOb 171SS8 NBSIR 82-2620 Annual Report 1982 Center for Analytical Chemistry U.S. DEPARTMENT OF COMMERCE National Bureau of Standards National Measurement Laboratory Washington, DC 20234 October 1982 Final Issued December 1982 QC 100 U56 #82-2620 1982 C . 2 Prepared for U.S. DEPARTMENT OF COMMERCE National Bureau of Standards Washington, DC 20234 NBSIR 82-2620 ANNUAL REPORT 1982 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 1982 Final Issued December 1982 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 , 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 7 C. Pilot National Environmental Specimen Bank Program 10 D. Service Analysis 21 E. Laser Analytical Chemistry Group 23 1. Group Overview 23 2. Selected Technical Reports 24 a. Computer Simulation of Charge Transport and Current Detection Following Ionization in Flames. 24 b. Characterization of Pulsed LEI Current Detection and Implications for Analytical Measurements. ... 26 c. Stark Modulated Infrared Diode Laser Spectroscopy 30 d. Measurement of the Isotopic Ratios: 12 C/ 13 C and 14 15 N/ N 33 3. Outputs and Interactions 34 II. INORGANIC ANALYTICAL RESEARCH DIVISION A. Division Overview 37 B. Selected Technical Accomplishments 47 1. High-Accuracy pH Measurements 47 2. Resonance Ionization Mass Spectrometry of Vanadium, Molybdenum, and Rhenium 48 3. Depth Profiling of Bismuth in Silicon and Tin with Low-Energy Neutrons 51 4. Determination of Provenience of Artifacts with Lead Isotope Ratio Measurements 54 5. Treatment of Sources of Variability in the Inductively Coupled Plasma (ICP) Technique 56 6. Effect of Natural Isotopic Variability on Accurate Determination of Sulfur by Neutron Activation Analysis 58 7. Application of ID/MS to the Determination of sulfur in Biological and Environmental Standards 60 8. Development of a Laser Mass Spectrometry Laboratory. 62 9. Design and Construction of a Modern Facility for the Production of Ultrapure Reagents 64 10. Improved Procedure for the Determination of Cyanide by Ion Chromatography with Electrochemical Detection . 65 11. Direct Determination of Calcium in Urine Using a Thermally-Regulated D.C. PI asma-Echel le Spectrometer 66 12. Determination of Ultratrace Concentrations of Chromium by Isotope Dilution Mass Spectrometry 67 i Page 13. Improved Radiochemical Procedures for High Sensitivity Measurements of Ultratrace Concentrations of Tin and Mercury 68 14. Isotopic Fractionation of Gallium on an Ion Exchange Column 69 15. Improved Sensitivity in Instrumental Activation Analysis Using the Compton Suppression Technique .... 70 16. Development of an Isotope Dilution Mass Spectro- metric Procedure for Iodine in Botanical Materials ... 72 17. Ion Optics of Magnetic Sector Mass Spectrometers .... 73 18. The Use of a Chromium Internal Standard for the Analysis of Diverse Iron-Chromium-Nickel Alloys 75 19. Development of a Precise Static Leach Test and the Evaluation of Simulated Nuclear Waste Glasses for a Reference Material 77 20. New Concepts in the Design and Fabrication of Fluorescent Glass Standards for Use in Nondestructive Crack Testing 78 21. Characterization of Selected Trace Elements in the Chesapeake Bay 79 22. Research to Develop Isotope Dilution Mass Spectrometry for Ultratrace Concentrations of Cadmium 84 23. The Use of Round Robins to Evaluate State-of-the-Art Uranium and Plutonium Measurements by Thermal Ionization Mass Spectrometry 85 24. Standard Reference Materials 87 C. Outputs and Interactions 90 III. ORGANIC ANALYTICAL RESEARCH DIVISION A. Division Overview 105 B. Selected Technical Accomplishments 119 1. The Effect of C 18 Surface Coverage on Selectivity in Reversed-Phase HPLC 119 2. Determination of Ambient Temperature Vapor Pressures of Polycyclic Aromatic Hydrocarbons 123 3. Determination of Polycyclic Aromatic Hydrocarbons in Complex Mixtures Using HPLC with Mobile Phase and Fluorescence Wavelength Programming 125 4. Vidicon Based Fluorescence Detection for Qualitative and Quantitative Analyses in HPLC 128 5. Certification of SRM 1649, Urban Dust/Organics, for Selected Polycyclic Aromatic Hydrocarbons 129 6. Determination of Nitro-Polycycl ic Aromatic Hydro- carbons Using Post-Column Reduction to Fluorescent Amino Derivatives ^1 7. Methods for the Determination of Vitamins in Milk. 135 8. Certification of an SRM for the Anticonvulsant Drugs Carbamazepine and Valproic Acid in Serum 137 Page 9. Research Results on the Analysis of Polychlorinated Biphenyls in Oils 139 10. Analysis of a California State Reference Material for Pesticides in Sediments 142 11. Design and Construction of a Sampling System for Woodburning Stove Gases and Particulate Samples 143 12. Development of Methods for the Determination of Toxic Organic Compounds in Aqueous Leachates of Hazardous Wastes and Development of a Quality Assurance Sludge Material 144 13. GC/MS Determination of Acidic and Basic Compounds in a Shale Oil Process Water 148 14. Development of an Isotope Dilution/Mass Spectrometric Definitive Method for the Determination of Serum Urea. 150 15. Improved Instrumentation for Organic Isotope Dilution/Mass Spectrometry Measurements 153 16. Preparation of Solutions of Stable Isotope Labeled Marker Compounds for Use in the Analysis of Priority Pollutants 156 17. Surface-Enhanced Raman Spectroscopy of N-Methyl- pyridinium Cation and Pyridine: Identification of Surface Species 158 18. Electrochemical and Spectroelectrochemical Studies of Copper and Iron Bleomycin Complexes 159 19. Polymer Modified Electrodes: Electrocatalytic Sensors for Detection of Organic Analytes 160 20. Theoretical Analysis of Charge Transport in Polymer-Modified Electrodes 161 21. Characterization of an Angiotensin I SRM by Proton NMR Spectroscopy at 400 MHz 163 22. The Synthesis, Purification, and Characterization of 2-Methyl thio-oxazol ine Derivatives of Pentoses and Hexoses 166 23. An Efficient Two-Step Synthesis of a Novel 15 N-Labeled Cyclonucleotide: 2,3'-Anhydro-l-$-D- 15 fructofuranosyluracil- N -l ,6 ' -diphosphate 168 2 ' 24. Confirmation of the Standard Wavelength for the 100 °S Point of the International Sugar Scale by Polarimetric Measurements with a Dye Laser 172 25. Implementation of and Initial Research in Two-Dimensional Electrophoresis for Protein Separations 174 26. Total Protein Content Certification of SRM 909, Human Serum 175 27. Construction of a Toxic Chemicals Handling Laboratory 175 C. Outputs and Interactions 177 Page IV. GAS AND PARTICULATE SCIENCE DIVISION A. Division Overview 191 B. Selected Technical Accomplishments 199 1. Isotopic Abundance Measurements with the Laser Microprobe Mass Analyzer 199 2. Microbeam Analysis of Diffusion — Induced Grain Boundary Migration 201 3. Electron Beam Broadening in Thin Films of Uranium Alloys Analyzed in the Analytical Electron Microscope. 204 4. Status of the Quantitative Electron Probe Microanalysis Programs FRAME and FRAME C 205 5. Crystallographic Contrast in Ion Microprobe Analysis of Inconel 206 6. Development of a Comprehensive Algorithm to Calculate the Spectral Output Distribution of X-Ray Tubes for X-Ray Spectrometry 208 7. Certification of Thin-glass Films as Standard Reference Materials for X-ray Spectrometry and Microanalysis 209 8. X-Ray Spectrometri c Analysis of NBS-SRM Bovine Liver and Pine Needles After Separation and Preconcentration 211 9. Evaluation of Personal Monitors 213 10. Measurement of the Temperature Dependence of the Ozone Absorption Cross-Section in the Ultraviolet. 216 11. Completion of Reference Ultraviolet Photometer for Ozone Calibrations 216 12. Photoacoustic Detection of HC1 217 13. A Study of Measurement Interference In The Photoacoustic Detection of N02 by Argon-Ion Laser Excitation 219 14. Accelerator Mass Spectrometry (AMS) 222 15. Receptor Modeling and Radiocarbon in Aerosols: Source Apportionment 224 16. Methodology for Vapor Pressure Measurements of Organics in the 10 to 10~ 5 Pascal Range 226 17. Development of Multicomponent Toxic Organics-in-Ai r Standards 228 18. Standards for Measurement of Atmospheric Carbon Dioxide 229 19. Development of Protocols for Providing Traceability of Commercial Gas Standards to NBS SRM Gas Mixtures. 231 20. Design and Evaluation of a High-Rate Passive Sampler for Ambient Levels of Nitrogen Dioxide 234 36 40 21. Development of Mixtures of Ar and Ar for Characterization of the Atmosphere of Venus 236 22. Development of Parts-per-Bi 1 1 ion Nitrous Oxide-in-Air Standard Reference Materials 237 C. Outputs and Interactions 240 IV 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
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