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Technical Activities 1985: Center for Analytical Chemistry REFERENCE NBSIR 85-3272 NBS PUBLICATIONS echnical Activities 1985 Genter for Analytical Chemistry -QC 100 November 1985 - U 5 6 U.S. DEPARTMENT 85-3272 OF COMMERCE National Bureau of Standards 1985 NBS RESEARCH NBSIR 85-3272 INFORMATION CENTER Center for Analytical Chemistry Richard A. Durst Harry S. Hertz John K. Taylor U.S. DEPARTMENT OF COMMERCE National Bureau of Standards National Measurement Laboratory Center for Analytical Chemistry Gaithersburg, MD 20899 November 1985 U.S. DEPARTMENT OF COMMERCE, Malcolm Baldrige. Secretary National Bureau of Standards, Ernest Ambler Director TABLE OF CONTENTS Page I. CENTER FOR ANALYTICAL CHEMISTRY A. Center Overviews 1 B. Output and Interactions 13 C. Voluntary Standardization and Quality Assurance 19 1. Voluntary Standards 19 2. Quality Assurance 19 D. Service Analysis 21 II. INORGANIC ANALYTICAL RESEARCH DIVISION A. Division Overviews 22 B. Selected Technical Reports 32 1. Three-Dimensional Atomic Sepectra in Flames Using Stepwise Excitation Laser-Enhanced Ionization Spectroscopy 32 2. Evaluation of Several Pulsed Dye Lasers as Excitation Sources for Flame Atomic Fluorescence Spectrometry 33 3. Determination of Cr(VI) in Natural Waters by LC/AAS after Separation and Preconcentration 34 4. Development of an SRM to Calibrate Microspectrofluorimeters 35 5. Spectrometric Analysis of Spark-Generated Aerosols 35 6. Resonant Laser^-Induced Ionization of Atoms in an Inductively-Coupled Plasma 37 7. An X-Y Scanning Photometer for Verifying the Transmittance Uniformity of Solid Filter SRMs 37 8. Statistical Ruggedness Testing of Acid Rain pH Measurements 38 9. Improvements in the Determination of Sulfide by Ion Chromatography 39 10. Direct Microwave Coupling Closed-Vessel Acid Dissolution 40 11. Leaching of Trace Metals from High Purity Fluor opolymers 41 12. Development of an Electrometer for Use with Thermal Ionization Mass Spectrometers 42 13. Determination of the Lead Isotopic Composition in Human Blood from the Italian Isotopic Lead Experiment.. 43 14. Studies on Ion Optics - Stray Fields 44 15. Automation of RIMS 45 16. Methodology Development for Sub-ppm Boron Measurements 46 17. Time-Resolved, Magnetic-Dispersion for Large Isotope Ratio Measurements By Resonance Ionization Mass Spectrometry (RIMS) 47 18. A New Method for the Accurate and Precise Determination of Se at Nanogram Levels 48 19. The Determination of Iodine in Foods and Other Biological Materials by Epithermal Neutron Activation Analysis 49 20. Multielement Analysis of Biological Macromolecules iii TABLE OF CONTENTS (Continued) Page 21. Light Element Determination by Neutron Activation Analysis 51 22. Neutron Depth Profiling: Industrial Interaction and Application 52 23. Re-Characterization of the NBSR at 20 MW 53 24. Determination of Gold and Platinum in Urine at Picogram Concentrations 54 25. Optimized Measurement of Iodine Isotopic Ratio by Neutron Activation 55 26. Laboratory Information Management Systems (LIMS) 57 27. Development of a Standard Reference Material for Rainwater Analysis 57 28. Standard Reference Materials 58 C. Outputs and Interactions 62 III. ORGANIC ANALYTICAL RESEARCH DIVISION A. Division Overview 81 B. Selected Technical Reports 95 1 . Investigations of Substrate Morphology in Chromatographic Sorbents by Small-Angle Neutron Scattering 95 2. Investigation of Secondary Chemical Equilibria in Liquid Chromatography: Verification of Optimization Theory for Acid-Base Equilibria and Identification of Factors which Influence Self-Selectivity 96 3. Optimization of Selectivity Using Sequentially Coupled Capillary Gas Chromatographic Columns 97 4. On-Line Two-Dimensional Chromatography Using Supercritical Carbon Dioxide as a Mobile Phase 99 5. Development of a Supercritical Extraction Procedure for the Removal of Trace Organic Species from Solid Samples 99 6. Development of a Method for the Stabilization of Ascorbic Acid in Solution and in Human Serum 100 7. Investigations of the Stability and Recovery of Toxic Organic Gases Adsorbed on Tenax 101 8. Design and Implementation of a Comprehensive Laboratory Information Management System to Acquire, Manipulate, and Archive Chromatographic Data Bases 102 9. Photodissociation of Ions Generated by Cesium Ion Bombardment for Determination of the Structures of Organic Molecules 103 10. Comparison of Two Methods for the Calibration of Gas Chromatography/Mass Spectrometry Instrumentation Used for the Analysis of Volatile Organic Compounds 104 11. Comparison of the College of American Pathologists Proficiency Testing Program Results and NBS Definitive Method Results for Four Organic Analytes in Serum 105 12. Stabilization of Polymer-Film Electrode Morphology by Thermal and Photochemical Crosslinking 106 IV 3 TABLE OF CONTENTS (Continued) Page 1 . Polyvinylf errocene-Modif ied Reference Electrode for Nonaqueous Electrochemistry 107 14. Investigation of the Electrochemical Behavior of Metal-Dithiolene Complexes 109 15. Investigation of the Electro-oxidative Products of Retinol and B-Carotene 110 16. Development of Two-Dimensional DEPT CH J-Resolved 1 ^C NMR Spectrum Editing Ill 17. Investigation of Metal-Protein Interactions 18. Viral Proteins from Vaccine Studied by Two-Dimensional Electrophoresis 112 19. Proteins from Honey Differential by Ultra-Thin Isoelectric Focusing and Two-Dimensional Electrophoresis 113 20. Results from Interlaboratory Analyses of Vitamins and Trace Metals 113 21. Preparation and Certification of Standard Reference Materials for Dioxins, Chlorinated Pesticides and PCBs 114 22. Certification of Standard Reference Material 1587 Nitrated Polycyclic Aromatic Hydrocarbons in Methanol 117 23. NBS Participation in the Certification of a Canadian Marine Sediment Reference Material 118 C. Outputs and Interactions 119 IV. GAS AND PARTICULATE SCIENCE DIVISION A. Division Overview 132 B. Selected Technical Reports 145 1. Development of Ultra-Trace (1 ppb) and SRM Multi-Component Toxic Organic Gas Standards 145 2. Sampling and Analysis of Nitrous Oxide, Carbon Dioxide, and Methane to Characterize Nitrogen and Carbon Cycles During NITROP-85 Cruise in the Peru Coastal Upwelling Region 146 3. Application of Electrochemical Methods for the Absolute Measurement of SO SRMs 2 Gas 147 4. Measurement of Nitric Acid in High Concentration N0 2 SRMs Using Diode Laser Spectroscopy Coupled with Chemiluminescence Analysis 148 5. Development of New SRMs for C0 in Air at Atmospheric 2 Concentrations for World-Wide Monitoring of Atmospheric C0 Changes 2 149 6 . Indoor Air Measurements for Sulfur Dioxide, Nitrogen Oxides, and Ozone in the National Library of Medicine.. 149 7. Development of NBS Traceable Standards for Measurements of U.S. Natural Gas Quality 150 8 . Development of Tritiated Methane Standards for Atmospheric Monitoring 1 51 v 1 TABLE OF CONTENTS (Continued) 9. Page Characterization of Stable NBS Traceable Standards of SO in Air at 100 ppb for Dry Acid Deposition Studies.. 2 152 10. Intercomparison of Tunable Diode Laser, Chemiluminescent Detector, and Fourier Transform IR Measurements of High Concentration NOj/Air SRMs 153 11. Identification and Characterization of Systematic Error Sources in Tunable Diode Laser Absorption Measurements 154 12. The Investigation of Simulated Test Data (STD) for Basic Research and Accuracy Evaluation in Chemometrics 155 13. Improved Measurements of Environmental Radiocarbon via Chemical and Isotopic Separation Coupled to Accelerator Mass Spectrometry 156 14. Carbon Isotope Measurements for Source Apportionment of Pollutant Aersols and Gases 157 15. Quantitative Compositional Mapping with the Electron Microprobe Using Wavelength and Energy Dispersive Techniques 159 16. Development of New Techniques for Light Element and Trace Element Compositional Mapping. 160 17. Determination of the Half-Life of '°^Re by Laser Microprobe Mass Spectrometry for Geochemical Dating.... 1 6 18. Unique Molecular Characterization of Complex Minerals by Micro-Raman Spectroscopy 161 19. Development of Digital Imaging on the Analytical Electron Microscope 162 20. The Development of a Particle Collector for Microanalysis of Fine Particulate Matter 1 63 21 . The Determination of the Visibility of Chrysotile Asbestos Fibers Imaged in the Scanning Electron Microscope 164 22. Magnification Calibration of the Scanning Transmission Electron Microscope by Hough-Transformed Images of Grating Replicas 165 23. A Comparison of Two Transient Recorders for Use with The Laser Microprobe Mass Analyzer 166 24. Automated Method for Analyzing Images Containing Electron Diffraction Spots 167 25. Determination of the Radiation Damage to Polycarbonate Film SRMs Used in X-Ray Spectrometry 168 26. Improvements in NBSGSC - A Fortran Program for Quantitative X-Ray Fluorescence Analysis 169 C. Outputs and Interactions 171 vi . I. Center for Analytical Chemistry Harry S. Hertz, Director Richard A. Durst, Acting 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 reference materials and provision of measurement services in the field of analytical chemistry. Analytical measurements provide a foundation for scientific and technological research and development concern- ing materials and their practical application. Moreover, analytical measure- ments are increasingly used as the basis for industrial, regulatory, and health-related decisions. The Center serves
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