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Center for Analytical Chemistry NBS PUBLICATIONS A111D4 0 7 b 5 b b NBSIR 84-2979 Technical Activities 1984 Center for Analytical Chemistry R. A. Velapoldi, H. S. Hertz, and J. K. Taylor U.S. DEPARTMENT OF COMMERCE National Bureau of Standards National Measurement Laboratory Gaithersburg, MD 20899 October 1984 Final Issued December 1984 Prepared for U.S. DEPARTMENT OF COMMERCE -QC National Bureau of Standards 100 Gaithersburg, MD 20899 . U56 GO 4-2979 1934 c, 2 NATIONAL BUREAU OF STANDARDS LIBRARY NBSIR 84-2979 Crrc TECHNICAL ACTIVITIES 1984 D-Cttoo CENTER FOR ANALYTICAL CHEMISTRY R. A. Velapoldi, H. S. Hertz, J. K. Taylor U.S. DEPARTMENT OF COMMERCE National Bureau of Standards National Measurement Laboratory Gaithersburg, MD 20899 October 1 984 Final Issued December 1984 Prepared for U.S. DEPARTMENT OF COMMERCE National Bureau of Standards Gaithersburg, MD 20899 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. Voluntary Standardization and Quality Assurance 1C 1. Voluntary Standardization 10 2. Quality Assurance 10 C. Service Analyses 12 II. INORGANIC ANALYTICAL RESEARCH DIVISION A. Division Overviews 13 B. Selected Technical Accomplishments 24 1 . Determination of Boron in Borosilicate Glasses by Neutron Capture Gamma-Ray Activation Analysis 24 2. Neutron Depth Profiling: Development and Intertechnique Comparisons 24 3. High Accuracy Determination of ^ 35 u j n Nondestructive Assay Standards by Gamma-Ray Spectrometry 25 4. Accurate Multi-Element Analysis of an Aquatic Accumulator 26 5. High Repetition Rate Tunable Laser System for Atomic Spectroscopy 27 6. Development of a High Accuracy Spectrometer for Laser-Enhanced Ionization 27 7. The Determination of Nickel in Petroleum Products Using Laser-Enhanced Ionization Spectrometry 28 8. An Evaluation of the Long-Term Stability of NBS Glass and Thin Metal Film Transmittance SRM's .... 29 9. The Use of the Box Plot to Describe Heterogeneity of Iron Samples 29 10. Redetermination of the Atomic Weight of Gallium . 11. Flow-Injection for On-Line Standard Addition Calibration Using a Wavelength-Modulated DCP Spectrometer 31 12. Speciation of Tributyltin in Seawater 13. Physical and Chemical Properties of Aerosols Produced by the Spark Discharge 14. Characterization of Autoionizing Levels in Beryllium with Resonance Ionization Mass Spectrometry 3- 15. The Determination of Iron in Serum and Water by Resonance .Ionization Isotope Dilution Mass Spectrometry 16. High Precision Isotope Ratio of • . Measurements CO 2 • 17. Certification of Nuclear Isotopic Standard Reference Materials 18. Determination of Trace-Level Cr(VI) in the Presence of Cr(III) and Fe(III) by Voltammetric Flow- Injection Analysis 19. The Measurement of pH and Acidity in Rainwater: Development of a Research Material/Simulated Rainwater 1 TABLE OF CONTENTS (Continued) Page 20. Uranium and Sulfur Isotopic Tracers in the Environment 39 21 . Standard Reference Materials 40 C. Outputs and Interactions 44 III. ORGANIC ANALYTICAL RESEARCH DIVISION A. Division Overview 61 B. Selected Technical Accomplishments 74 1 . Development of a Definitive Method for Serum Creatinine 74 2. Investigation of Factors Affecting the Selectivity of Negative Ion Chemical Ionization Mass Spectrometry for Isomeric Polynuclear Aromatic Hydrocarbons .... 75 3. Development of an Isotope Dilution GC/MS Procedure for Analysis of Toxic Organics in Air Mixtures 76 4. Photodissociation of Ions Generated by 'Soft Ionization Techniques 76 5. Investigation of Ion/Molecule Reactions in a Triple Quadrupole Mass Spectrometer 78 6. Analysis of the Proton and Carbon-13 NMR Spectra of Equilibrated Digitoxose by Two-Dimensional, Chemical Shift Correlation Methods 79 7. Identification of Metal Binding Proteins in Polyacrylamide Gels by Neutron Activation Studies 80 8. Squid Species Differentiated by Use of Thin Layer Isoelectric Focusing 81 9. Determination of Pesticides and PCBs in Cod-Liver Oil 81 10. Determination of Dioxin in Soils 82 1 1 . Development of a Laboratory Data Networking System . 83 12. Research on Metal Chelate Columns 84 13. Influence of Physical and Chemical Parameters of Silica Substrates on the Reversed-Phase Liquid Chromatographic Performance of Alkyl Bonded Phases 85 14. Optimization of Secondary Chemical Equilibria in Liquid Chromatography 86 15. Quantitative Analysis of Complex Mixtures by LC/MS/MS 87 16. Thermal Crosslinking Procedure for Preparing Solvent-Stable Polymei—Film Electrodes 88 17. Electrocatalytic Reduction of Ethylene Dibromide via Rhodium(II) Tetraphenylporphyr in Dimer Derivatized Polymer Film Electrodes 89 18. Refinement of the Mathematical Model for Charge Transport in Polymer-Film Electrodes 90 19. Electrochemical Characteri zation of a Series of Metal-Di thiosquarate Complexes 91 TABLE OF CONTENTS (Continued) Page 20. Preparation and Characterization of Reference Materials for EPA's Water and Hazardous Waste Program 91 21 . Certification of a Priority Pollutant Phenols in Methanol SRM 93 22. Certification of a Diesel Particulate SRM 93 23. Certification of a Gas Chromatography/Mass Spectrometry Performance SRM 95 C. Outputs and Interactions 96 IV. GAS AND PARTICULATE SCIENCE DIVISION A. Division Overview 108 B. Selected Technical Accomplishments 119 1 . Development of an Accurate Calibration Standard for the Measurement of Atmospheric Tritium 119 2. Assessment of Uncertainties in Gravimetrically- Prepared Toxic Organic Gas Mixtures in the Part- Per-Billion Range 120 3. Measurements of the Temperature Dependence of Selected Infrared Band Strengths of Halocarbons F-11 (CC1 F) and F-12 (CC1 F ) 121 3 2 2 4. Development of a Cryogenic Preconcentration Technique for the Analysis of Ultratrace Constituents in Gas Mixtures 122 5. The Investigation of the Long-Term Stability of Tetrachloroethylene Permeation Tubes 122 6. Development of an Improved Methanation System for the Analysis of CO and C0 2 SRM’s 123 7. The Development of a System for Analytical Traceability in the State Motor Vehicle Emissions Testing Program 124 8. Advances in Carbon Isotopic Ratio Measurements by Accelerator Mass Spectrometry 125 9. Development of a Definitive Treatment for the Calculation of Lower Limits of Detection in Radionuclide Monitorings 126 10. A System for Traceable Calibration of Ozone 12" Measurements Using the NBS Primary Ozone Photometer . 11. Research in Measurement Methodology Using Diode Laser Spectrometry and the Determination of Spectroscopic and Kinetic Data for Reactive Atmospheric Molecules 12" 12. Development of an Improved Procedure to Calculate Characteristic X-ray Fluorescence Corrections from an Electron Microprobe *2“ 13. Development of an Automated Digital Image Acquisition System for Analytical Electron Microscopy ' - 14. Comparison of Boron-10 Depth Distributions as Determined by Spreading Resistance, Secondary Ion Mass Spectrometry , and Neutron Depth Profiling .... i i i TABLE OF CONTENTS (Continued) Page 15. Development of Improved Elemental and Isotopic Measurements of Micrometer Sized Particles by Secondary Ion Mass Spectrometry 131 16. Evaluation of a Digital Image Analysis System for the Secondary Ion Microanalyzer 132 17. Automated Object Identification From Digital Images . 133 18. The Detection and Identification of Surface Organic Species by Laser Ionization Mass Spectrometry 133 19. Comparison of Multichannel SIT Vidicon and Monochannel Photomultiplier Detection in Micro- Raman Spectroscopy 13^ 20. The Certification of New Multielement Glass Standards For Analytical Microprobes 135 21. The Analysis of Natural Product SRM's by X-ray Fluorescence 136 22. Improvements in the Algorithm for Calculating Fundamental Parameters in Quantitative X-ray Fluorescence Analysis 135 C. Outputs and Interactions 138 IV . I. Center for Analytical Chemistry Harry S. Hertz, 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 reference materials and provision of measurement services, in the field of analytical chemistry. Analytical measurements provide a foundation for scientific and technological research and develop- ment concerning materials and their practical application. Moreover, analyti- cal measurements are increasingly used as the basis for industrial, regula- tory, and health-related decisions. The Center serves as the National Reference Laboratory for assuring the reliability of analytical measurements. The principal means by which the Center has served as a National Reference Laboratory is through the development of measurement concepts and methods, provision of quality assurance services, and certification 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 reference materials are widely used in such diverse areas as the metal and chemical industries and in clinical and environmental laboratories. Each standard is supported by research on homogeneity and stability and is certified as to chemical composition using the most reliable analytical methods available. Analytical chemistry is increasingly being called upon to provide key data for highly complex sample types - hazardous chemical and nuclear wastes, body fluids, plant
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