Principles and Practice of X-Ray Spectrometric Analysis

I. X-Ray Physics.- 1. Excitation and Nature of X-Rays; X-Ray Spectra.- 1.1. Historical.- 1.2. Definition of X-Rays.- 1.3. Properties of X-Rays.- 1.4. Units of X-Ray Measurement.- 1.4.1. Frequenc.- 1.4.2. Wavelengt.- 1.4.3. Energy.- 1.4.4. Intensity.- 1.5. The Continuous Spectrum.- 1.5.1. Nature.- 1.5.2. Generation.- 1.5.3. Short-Wavelength Limit.- 1.5.4. Origin of the Continuum.- 1.5.5. Effect of X-Ray Tube Current, Potential, and Target.- 1.5.6. Significance.- 1.6. The Characteristic Line Spectrum.- 1.6.1. Atomic Structure.- 1.6.2. Nature and Origin.- 1.6.2.1. General.- 1.6.2.2. Band Spectra.- 1.6.2.3. Selection Rules.- 1.6.2.4. Notation.- 1.6.2.5. Wavelength.- 1.6.2.6. Intensity.- 1.6.3. Excitation-General.- 1.6.4. Primary Excitation.- 1.6.5. Secondary Excitation.- 1.6.5.1. X-Ray Absorption Edges.- 1.6.5.2. Principles.- 1.6.5.3. Relationship of Absorption Edges and Spectral-Line Series.- 1.6.5.4. Excitation with Polychromatic X-Rays.- 1.6.5.5. Other Contributions to the Specimen Emission.- 1.7. Comparison of Primary and Secondary Excitation.- 1.7.1. X-Ray Tube Potential.- 1.7.2. Features.- 1.8. Excitation by Ion Bombardment.- 2. Properties of X-Rays.- 2.1. Absorption.- 2.1.1. X-Ray Absorption Coefficients.- 2.1.2. X-Ray Absorption Phenomena.- 2.1.3. Relationship of ??, ?, and Z.- 2.1.4. Absorption Edges.- 2.1.5. Comparison of X-Ray and Optical Absorption.- 2.1.6. Significance.- 2.1.7. Half-Thickness and Absorption Cross Section.- 2.1.8. Inverse-Square Law.- 2.2. Scatter.- 2.2.1. General.- 2.2.2. Modified (Compton) Scatter.- 2.2.3. Relationship of Unmodified and Modified Scatter.- 2.2.4. Significance.- 2.3. Diffraction by Crystals.- 2.4. Specular Reflection; Diffraction by Gratings.- 2.4.1. Specular Reflection.- 2.4.2. Diffraction by Gratings.- 2.5. Auger Effect; Fluorescent Yield.- 2.5.1. Auger Effect.- 2.5.2. Fluorescent Yield.- 2.5.3. Satellite Lines.- II. The X-Ray Spectrometer, its Components, and their Operation.- 3. X-Ray Secondary-Emission (Fluorescence) Spectrometry; General Introduction.- 3.1. Nomenclature.- 3.2. Principle and Instrument.- 3.2.1. Principle.- 3.2.2. The X-Ray Spectrogoniometer.- 3.2.3. Electronic Readout Components.- 3.2.4. Qualitative, Semiquantitative, and Quantitative Analysis.- 3.2.5. Phases of a Quantitative X-Ray Spectrometric Analysis.- 3.3. Appraisal.- 3.3.1. Advantages.- 3.3.1.1. X-Ray Spectra.- 3.3.1.2. Excitation and Absorption.- 3.3.1.3. Absorption-Enhancement Effects.- 3.3.1.4. Spectral-Line Interference.- 3.3.1.5. Nondestruction of Specimen.- 3.3.1.6. Specimen Versatility.- 3.3.1.7. Operational Versatility.- 3.3.1.8. Versatility of Analytical Strategy.- 3.3.1.9. Selected-Area Analysis.- 3.3.1.10. Semiquantitative Estimations.- 3.3.1.11. Concentration Range.- 3.3.1.12. Sensitivity.- 3.3.1.13. Precision and Accuracy.- 3.3.1.14. Excitation.- 3.3.1.15. Speed and Convenience.- 3.3.1.16. Operating Cost.- 3.3.1.17. Automation.- 3.3.1.18. Process Control.- 3.3.1.19. Use with Other Methods.- 3.3.2. Disadvantages.- 3.3.2.1. Light Elements.- 3.3.2.2. Penetration.- 3.3.2.3. Absorption-Enhancement Effects.- 3.3.2.4. Sensitivity.- 3.3.2.5. Qualitative Analysis.- 3.3.2.6. Standards.- 3.3.2.7. Instrument Preparation.- 3.3.2.8. Components.- 3.3.2.9. Instrument Settings.- 3.3.2.10. Error.- 3.3.2.11. Tedium.- 3.3.2.12. Cost.- 3.4. Trends in X-Ray Spectrochemical Analysis.- 4. Excitation.- 4.1. Principles.- 4.1.1. General.- 4.1.2. Excitation by Monochromatic X-Rays.- 4.1.3. Excitation by Continuous Spectra.- 4.2. The X-Ray Tube.- 4.2.1. Function and Requirements.- 4.2.2. Construction.- 4.2.3. Design Considerations.- 4.2.4. Practical Considerations.- 4.2.4.1. Excitation Efficiency.- 4.2.4.2. Spectral-Line Interference.- 4.2.4.3. Temperature.- 4.2.4.4. Evaluation of the Condition of the X-Ray Tube.- 4.2.5. Special X-Ray Tubes.- 4.2.5.1. Dual-Target Tube.- 4.2.5.2. End-Window Tube.- 4.2.5.3. Demountable Tubes.- 4.2.5.4. Tubes for Ultralong Wavelength.- 4.2.5.5. Low-Power Tubes.- 4.2.5.6. Field-Emission Tubes.- 4.3. X-Ray Power Supply.- 4.3.1. Function and Requirements.- 4.3.2. Components and Operation.- 4.3.2.1. High-Potential Supply.- 4.3.2.2. X-Ray Tube Filament Supply.- 4.3.2.3. Operation.- 4.3.2.4. Stabilization.- 4.3.2.5. Safety and Protective Devices.- 4.3.3. Practical Considerations.- 4.3.3.1. Constant Potential.- 4.3.3.2. Maximum Target Potential.- 4.3.3.3. Operating Conditions.- 4.4. Filters in Secondary Excitation.- 4.4.1. Attenuation Filters.- 4.4.2. Enhancement Filters.- 4.4.3. Enhancement Radiators.- 4.5. Specimen Presentation.- 5. Dispersion.- 5.1. Introduction.- 5.2. Collimators.- 5.2.1. Function.- 5.2.2. Features and Considerations.- 5.3. Radiation Path.- 5.4. Analyzer Crystals.- 5.4.1. Introduction.- 5.4.2. Features.- 5.4.2.1. Wavelength Range.- 5.4.2.2. Diffracted Intensity.- 5.4.2.3. Resolution.- 5.4.2.4. Peak-to-Background Ratio; Crystal Emission.- 5.4.2.5. Thermal Expansion.- 5.4.2.6. Miscellaneous Features.- 5.4.2.7. Aligning and Peaking the Goniometer.- 5.4.3. Other Dispersion Devices.- 5.4.3.1. Gratings and Specular Reflectors.- 5.4.3.2. Multilayer Metal Films.- 5.4.3.3. Metal Disulfide-Organic Intercalation Complexes.- 5.4.3.4. Multilayer Soap Films.- 5.4.3.5. Pyrolytic Graphite.- 5.5. Basic Crystal-Dispersion Arrangements.- 5.5.1. Multichannel Spectrometers.- 5.5.2. Flat-Crystal Dispersion Arrangements.- 5.5.2.1. Bragg and Soller.- 5.5.2.2. Edge-Crystal.- 5.5.2.3. Laue.- 5.5.2.4. Other Flat-Crystal Arrangements.- 5.5.3. Curved-Crystal Dispersion Arrangements.- 5.5.3.1. General.- 5.5.3.2. Transmission.- 5.5.3.3. Reflection.- 5.5.3.4. Von Hamos Image Spectrograph.- 5.6. Curved-Crystal Spectrometers.- 5.6.1. Semifocusing Spectrometer.- 5.6.2. Continuously Variable Crystal Radius.- 5.6.3. Naval Research Laboratory Design.- 5.6.4. Applied Research Laboratories Design.- 5.6.5. Cauchois Spectrometer.- 5.6.6. Spherically Curved-Crystal Spectrometers.- 5.7. Photographic X-Ray Spectrographs.- 6. Detection.- 6.1. Introduction.- 6.2. Gas-Filled Detectors.- 6.2.1. Structure.- 6.2.1.1. Components, Classifications.- 6.2.1.2. Windows.- 6.2.1.3. Gas Fillings.- 6.2.2. Operation.- 6.2.2.1. Phenomena in the Detector Gas Volume.- 6.2.2.2. Proportionality in Gas Detectors.- 6.2.2.3. Gas Amplification; Types of Gas Detectors.- 6.2.2.4. Quenching.- 6.2.3. Proportional Counters.- 6.2.3.1. Phenomena in the Detector Gas Volume.- 6.2.3.2. Detector Output; Escape Peaks.- 6.3. Scintillation Counters.- 6.3.1. Structure.- 6.3.1.1. Scintillation Crystal.- 6.3.1.2. Multiplier Phototube.- 6.3.2. Operation.- 6.3.2.1. Proportionality in Scintillation Counters.- 6.3.2.2. Phenomena in the Scintillation Counter.- 6.4. Lithium-Drifted Silicon and Germanium Detectors.- 6.4.1. Structure.- 6.4.2. Operation.- 6.4.3. Advantages.- 6.4.4. Limitations.- 6.4.5. Avalanche Detectors.- 6.5. Evaluation of X-Ray Detectors.- 6.5.1. Detector Characteristics.- 6.5.1.1. Rise Time.- 6.5.1.2. Dead Time.- 6.5.1.3. Resolving Time.- 6.5.1.4. Recovery Time.- 6.5.1.5. Linear Counting Range.- 6.5.1.6. Coincidence Loss.- 6.5.1.7. Choking.- 6.5.1.8. Plateau.- 6.5.1.9. Slope.- 6.5.1.10. Inherent Noise and Background.- 6.5.1.11. Quantum Efficiency.- 6.5.1.12. Resolution.- 6.5.2. Comparison of Conventional Detectors.- 6.5.3. Modified Gas-Filled and Scintillation Detectors.- 6.6. Other X-Ray Detectors.- 6.6.1. Photographic Film.- 6.6.2. Photoelectric Detectors.- 6.6.2.1. The Phosphor-Phototube Detector.- 6.6.2.2. Photoelectric Detectors for the Ultralong-Wave-length Region.- 6.6.3. Crystal Counters.- 7. Measurement.- 7.1. Instrumentation.- 7.1.1. Introduction.- 7.1.2. Preamplifier.- 7.1.3. Amplifier.- 7.1.4. Pulse-Height Selectors.- 7.1.4.1. Pulse-Height Selector; Discriminator.- 7.1.4.2. Pulse Reverter.- 7.1.4.3. Pulse-Shape Selector.- 7.1.5. Ratemeter and Recorder.- 7.1.6. Scaler and Timer.- 7.1.7. Computers.- 7.2. Measurement of Intensity.- 7.2.1. Ratemeter Methods.- 7.2.2. Scaler-Timer Methods.- 7.2.2.1. Preset-Time Method.- 7.2.2.2. Preset-Count Method.- 7.2.2.3. Integrated-Count Method.- 7.2.2.4. Monitor and Ratio Methods.- 7.2.3. X-Ray Dose and Dose Rate.- 7.3. Background.- 7.3.1. Definition and Significance.- 7.3.2. Origin and Nature.- 7.3.3. Measurement.- 7.3.4. Reduction.- 7.3.5. Considerations.- 8. Pulse-Height Selection; Energy-Dispersive Analysis; Nondispersive Analysis.- 8.1. Pulse-Height Selection.- 8.1.1. Principle of Pulse-Height Selection.- 8.1.2. Pulse-Height Distribution Curves.- 8.1.2.1. Introduction.- 8.1.2.2. Single-Channel Pulse-Height Selector.- 8.1.2.3. Multichannel Pulse-Height Analyzer.- 8.1.3. Pulse-Height Selector Displays.- 8.1.4. Pulse-Height Selector Operating Controls.- 8.1.5. Use of the Pulse-Height Selector.- 8.1.5.1. Evaluation of Detector and Amplifier Characteristics.- 8.1.5.2. Establishment of Pulse-Height Selector Settings.- 8.1.6. Applications and Limitations.- 8.1.7. Automatic Pulse-Height Selection.- 8.1.8. Problems with Pulse-Height Selection.- 8.1.8.1. General.- 8.1.8.2. Shift of Pulse-Height Distribution.- 8.1.8.3. Distortion of Pulse-Height Distribution.- 8.1.8.4. Additional Pulse-Height Distributions Arising from the Measured Wavelength.- 8.1.9. Unfolding of Overlapping Pulse-Height Distributions.- 8.1.9.1. Principle.- 8.1.9.2. Application.- 8.1.9.3. Simplified Variations.- 8.2. Energy-Dispersive Analysis.- 8.2.1. Introduction.- 8.2.1.1. Principles.- 8.2.1.2. Advantages.- 8.2.1.3. Limitations.- 8.2.2. Instrumentation.- 8.2.2.1. General.- 8.2.2.2. Excitation by X-Rays.- 8.2.2.3. Excitation by Radioisotopes.- 8.2.2.4. Energy-Dispersive Multichannel X-Ray Spectrometer Systems.- 8.2.3. Energy-Dispersive Diffractometry-Spectrometry.- 8.3. Nondispersive Analysis.- 8.3.1. Selective Excitation.- 8.3.2. Selective Filtration.- 8.3.2.1. Methods.- 8.3.2.2. X-Ray Transmission Filters.- 8.3.3. Selective Detection.- 8.3.4. Modulated Excitation.- 9. Laboratory, Automated, and Special X-Ray Spectrometers.- 9.1. Introduction.- 9.2. Laboratory X-Ray Spectrometers.- 9.2.1. General.- 9.2.2. Instrument Arrangements.- 9.2.3. Accessories.- 9.3. Automated X-Ray Spectrometers.- 9.3.1. General.- 9.3.2. Sequential Automatic Spectrometers.- 9.3.3. Simultaneous Automatic Spectrometers.- 9.3.4. "Slewing" Goniometers.- 9.4. Special X-Ray Spectrometers.- 9.4.1. Portable Spectrometer.- 9.4.2. Primary Excitation.- 9.4.3. Ultralong-Wavelength Spectrometry.- 9.5. X-Ray Safety and Protection.- III. Qualitative and Semiquantitative Analysis.- 10. Qualitative and Semiquantitative Analysis.- 10.1. General.- 10.2. Recording the Spectrum.- 10.3. Instrument Conditions.- 10.4. Identification of the Peaks.- 10.4.1. Spectral-Line Tables.- 10.4.2. Identification of Peaks.- 10.5. General Procedures for Qualitative and Semiquantitative Analysis.- 10.5.1. Normalization Factor Method.- 10.5.2. Method of Salmon.- IV. Performance Criteria and other Features.- 11. Precision and Error; Counting Statistics.- 11.1. Error in X-Ray Spectrometric Analysis.- 11.1.1. Nature of Error.- 11.1.2. Elementary Statistics.- 11.1.3. Sources of Error.- 11.1.3.1. General.- 11.1.3.2. Instrumental and Operational Error.- 11.1.3.3. Specimen Error.- 11.1.3.4. Chemical Effects.- 11.2. Counting Statistics.- 11.2.1. Nature of the Counting Error.- 11.2.2. Calculation of Counting Error.- 11.2.2.1. Counting Error for Accumulated Counts.- 11.2.2.2. Counting Error for Intensities.- 11.2.3. Counting Strategy.- 11.2.3.1. Measurement of Net Intensity.- 11.2.3.2. The Ratio Method.- 11.2.4. Figure of Merit.- 11.3. Analytical Precision.- 11.3.1. Nature of Analytical Precision.- 11.3.2. Evaluation of Precision.- 11.3.2.1. General Considerations.- 11.3.2.2. Instrumental Instability.- 11.3.2.3. Operational Error.- 11.3.2.4. Specimen Error.- 11.3.2.5. Evaluation of Internal Consistency of Data.- 12. Matrix Effects.- 12.1. Introduction.- 12.2. Absorption-Enhancement Effects.- 12.2.1. General; Definitions.- 12.2.2. Effects on Calibration Curves.- 12.2.3. Prediction of Absorption-Enhancement Effects.- 12.2.3.1. K Lines.- 12.2.3.2. L Lines.- 12.2.4. Nonspecific Absorption Effects.- 12.2.5. Specific Absorption-Enhancement Effects.- 12.2.6. Secondary Absorption-Enhancement Effects.- 12.2.6.1. General.- 12.2.6.2. Secondary Absorption Effects.- 12.2.6.3. Secondary Enhancement Effects.- 12.2.7. Unusual Absorption-Enhancement Effects.- 12.3. Particle-Size, Heterogeneity, and Surface-Texture Effects.- 13. Sensitivity and Resolution; Spectral-Line Interference.- 13.1. Sensitivity.- 13.1.1. Definitions.- 13.1.2. Factors Affecting Sensitivity.- 13.1.2.1. Excitation Conditions.- 13.1.2.2. Specimen Conditions.- 13.1.2.3. Optical System.- 13.1.2.4. Detector and Readout Conditions.- 13.1.3. Photon Losses in the X-Ray Spectrometer.- 13.1.4. Sensitivity Performance.- 13.2. Resolution.- 13.2.1. Definitions.- 13.2.1.1. Resolution.- 13.2.1.2. Dispersion.- 13.2.1.3. Divergence.- 13.2.2. Factors Affecting Resolution.- 13.3. Spectral-Line Interference.- 13.3.1. Definition.- 13.3.2. Origin of Interfering Spectral Lines.- 13.3.2.1. Wavelength Interference.- 13.3.2.2. Energy Interference.- 13.3.2.3. Common Sources of Spectral Interference.- 13.3.3. Reduction of Spectral Interference.- 13.3.3.1. General Methods.- 13.3.3.2. Excitation of Analyte and Interferant Lines.- 13.3.3.3. Transmission and Detection of Analyte and Interferant Lines.- 13.3.3.4. Experimental and Mathematical Correction of Spectral Interference.- V. Quantitative Analysis.- 14. Methods of Quantitative Analysis.- 14.1. Introduction.- 14.2. Standard Addition and Dilution Methods.- 14.2.1. Principles and Considerations.- 14.2.2. Methods.- 14.2.2.1. Standard Addition.- 14.2.2.2. Standard Dilution.- 14.2.2.3. Multiple Standard Addition.- 14.2.2.4. Slope-Ratio Addition.- 14.2.2.5. Double Dilution.- 14.3. Calibration Standardization.- 14.3.1. Principles.- 14.3.2. Special Calibration Methods.- 14.3.2.1. Single-Standard Method.- 14.3.2.2. Two-Standard Method.- 14.3.2.3. Binary-Ratio Method.- 14.3.2.4. Mutual Standards Method.- 14.3.2.5. Sets of Calibration Curves.- 14.4. Internal Standardization.- 14.4.1. Principles.- 14.4.2. Selection of Internal-Standard Element.- 14.4.3. Advantages and Limitations.- 14.4.4. Considerations.- 14.4.5. Special Internal-Standardization Methods.- 14.4.5.1. Single-Standard Internal-Standard Method.- 14.4.5.2. Variable Internal-Standard Method.- 14.4.6. Other Standardization Methods.- 14.4.6.1. Internal Control-Standard Method.- 14.4.6.2. Internal Intensity-Reference Standard Method.- 14.4.6.3. External-Standard Method.- 14.5. Standardization with Scattered X-Rays.- 14.5.1. Background-Ratio Method.- 14.5.2. Graphic Method.- 14.5.3. Scattered Target-Line Ratio Method.- 14.5.4. Scattered Internal-Standard Line Method.- 14.5.5. Ratio of Coherent to Incoherent Scattered Intensities.- 14.5.6. Slurry-Density Method.- 14.6. Matrix-Dilution Methods.- 14.6.1. Principles.- 14.6.2. Discussion.- 14.7. Thin-Film Methods.- 14.7.1. Principles.- 14.7.2. Infinite (Critical) Thickness.- 14.7.3. Discussion.- 14.8. Special Experimental Methods.- 14.8.1. Emission-Absorption Methods.- 14.8.2. Method of Variable Takeoff Angle.- 14.8.2.1. Basic Excitation Equations.- 14.8.2.2. Evaluation of Mean Wavelength and Excitation Integral.- 14.8.2.3. Mass per Unit Area of an Element Film from Its Own Line.- 14.8.2.4. Mass per Unit Area of an Element Film from a Substrate Line.- 14.8.2.5. Mass per Unit Area and Composition of Multielement Films.- 14.8.2.6. Composition of Bulk Multielement Specimens.- 14.8.3. Indirect (Association) Methods.- 14.8.4. Combinations of X-Ray Spectrometry and Other Methods.- 15. Mathematical Correction of Absorption-Enhancement Effects.- 15.1. Introduction.- 15.2. Geometric Methods.- 15.3. Absorption Correction.- 15.4. Empirical Correction Factors.- 15.5. Influence Coefficients.- 15.5.1. Introduction.- 15.5.2. Derivation of the Basic Equations.- 15.5.2.1. Birks' Derivation.- 15.5.2.2. Muller's Derivation; Regression Coefficients.- 15.5.2.3. Influence Coefficient Symbols.- 15.5.3. Solution of the Basic Equations.- 15.5.3.1. Simplified Solutions.- 15.5.3.2. Evaluation of au Coefficients to a First Approximation.- 15.5.3.3. Evaluation of au Coefficients to a Second Approximation.- 15.5.3.4. Simultaneous Evaluation of All au Coefficients.- 15.5.3.5. Other Methods for Evaluation of au Coefficients.- 15.5.4. Variations of the Influence-Coefficient Method.- 15.5.4.1. Method of Sherman.- 15.5.4.2. Method of Burnham, Hower, and Jones.- 15.5.4.3. Method of Marti.- 15.5.4.4. Method of Traill and Lachance.- 15.5.4.5. Method of Lucas-Tooth and Pyne.- 15.5.4.6. Method of Rasberry and Heinrich.- 15.6. Fundamental-Parameters Method.- 15.7. Multiple-Regression Method.- VI. Specimen Preparation and Presentation.- 16. Specimen Preparation and Presentation-General; Solids, Powders, Briquets, Fusion Products.- 16.1. General Considerations.- 16.1.1. Introduction.- 16.1.2. Classification of Applications.- 16.1.3. Problems Specific to the Light Elements.- 16.1.4. Standards.- 16.1.4.1. General.- 16.1.4.2. Permanence of Standards.- 16.1.4.3. Sources of Standards.- 16.1.5. Effective Layer Thickness.- 16.1.6. The Specimen-Preparation Laboratory.- 16.2. Solids.- 16.2.1. Scope, Advantages, Limitations.- 16.2.2. Presentation.- 16.2.2.1. Flat Specimens.- 16.2.2.2. Fabricated Forms and Parts.- 16.2.3. Preparation.- 16.2.4. Precautions and Considerations.- 16.3. Powders and Briquets.- 16.3.1. Scope, Advantages, Limitations.- 16.3.2. Powder and Briquet Standards.- 16.3.3. Preparation of Powders.- 16.3.4. Presentation.- 16.3.4.1. Loose Powders.- 16.3.4.2. Briquets.- 16.3.4.3. Thin Layers.- 16.3.5. Precautions and Considerations.- 16.3.5.1. Particle-Size Effects.- 16.3.5.2. Additives.- 16.3.5.3. Briqueting.- 16.3.5.4. Other Considerations.- 16.4. Fusion Products.- 16.4.1. Scope, Advantages, Limitations.- 16.4.2. Materials.- 16.4.3. Specific Fusion Procedures.- 16.4.4. Considerations.- 17. Specimen Preparation and Presentation-Liquids; Supported Specimens.- 17.1. Liquid Specimens.- 17.1.1. Introduction.- 17.1.2. Advantages.- 17.1.3. Disadvantages.- 17.1.4. Liquid-Specimen Cells.- 17.1.4.1. Forms and Materials.- 17.1.4.2. General-Purpose Cell.- 17.1.4.3. Somar "Spectro-Cup".- 17.1.4.4. Cells for Use in Vacuum.- 17.1.4.5. Uncovered Cell.- 17.1.4.6. Frozen-Specimen Cell.- 17.1.4.7. Cell for Slurries.- 17.1.4.8. High-Temperature Liquid-Specimen Cell.- 17.1.4.9. Other Liquid-Specimen Cells.- 17.1.5. Precautions and Considerations.- 17.1.5.1. Interaction of the Primary Beam with Liquid Specimens.- 17.1.5.2. Composition.- 17.1.5.3. Miscellany.- 17.2. Supported Specimens.- 17.2.1. General.- 17.2.2. Specimens Derived from Liquids and Gases.- 17.2.3. Specimens Derived from Solids.- 17.2.4. Ion-Exchange Techniques.- 17.2.4.1. Principles.- 17.2.4.2. Techniques.- 17.2.5. Ashing Techniques.- 17.2.6. Bomb Techniques.- 17.3. Trace and Microanalysis.- 17.4. Radioactive Specimens.- VII. Unconventional Modes of Operation; Related X-Ray Methods of Analysis.- 18. Measurement of Thickness of Films and Platings.- 18.1. Principles and Basic Methods.- 18.2. Multiple-Layer and Alloy Platings.- 18.2.1. Multiple-Layer Platings.- 18.2.2. Alloy Platings-Composition and Thickness.- 18.3. Special Techniques.- 18.3.1. Special Specimen Forms.- 18.3.2. Selected-Area Analysis.- 18.3.3. Selective Excitation.- 18.3.4. Enhancement.- 18.3.5. Excitation by Radioactive Sources.- 18.3.6. Energy-Dispersive Operation.- 18.3.7. Decoration.- 18.3.8. Dynamic Studies.- 18.4. Considerations.- 19. Selected-Area Analysis.- 19.1. Principle and Scope.- 19.1.1. Principle.- 19.1.2. Applications.- 19.1.3. Advantages and Limitations.- 19.2. Selected-Area Analysis on Standard Commercial X-Ray Spectrometers.- 19.2.1. Specimen Irradiation.- 19.2.2. Selected-Area Apertures.- 19.2.2.1. General.- 19.2.2.2. Pinholes.- 19.2.2.3. Slits.- 19.2.2.4. Resolution.- 19.2.3. Dispersion.- 19.3. Instruments for Selected-Area X-Ray Spectrometric Analysis.- 19.4. Specimen Techniques.- 19.4.1. Preparation.- 19.4.2. Alignment of Selected Area and Aperture.- 19.5. Analytical Techniques.- 19.6. Performance.- 20. Other Analytical Methods Based on Emission, Absorption, and Scatter of X-Rays; Other Spectrometric Methods Involving X-Rays.- 20.1. X-Ray Absorption Methods.- 20.1.1. Polychromatic X-Ray Absorptiometry.- 20.1.1.1. Principles and Instrumentation.- 20.1.1.2. Advantages and Limitations.- 20.1.2. Monochromatic X-Ray Absorptiometry.- 20.1.2.1. Principles and Instrumentation.- 20.1.2.2. Advantages and Limitations.- 20.1.3. Applications of X-Ray Absorptiometry.- 20.1.4. X-Ray Absorption-Edge Spectrometry (Differential X- Ray Absorptiometry).- 20.1.4.1. Principles and Instrumentation.- 20.1.4.2. Advantages and Limitations.- 20.1.4.3. Applications.- 20.1.5. X-Ray Contact Microradiography.- 20.1.6. X-Ray Absorption-Edge Fine Structure.- 20.1.7. Specimen Preparation for X-Ray Absorption.- 20.2. X-Ray Scatter Methods.- 20.2.1. Coherent Scatter.- 20.2.2. Coherent/Incoherent Scatter Ratio.- 20.2.3. Determination of Dry Mass.- 20.3. Scanning X-Ray Microscopy.- 20.3.1. Introduction.- 20.3.2. Scanning X-Ray Emission Microscopy.- 20.3.3. Scanning X-Ray Absorption Microscopy.- 20.4. X-Ray Photoelectron and Auger-Electron Spectrometry.- 20.4.1. Introduction.- 20.4.2. X-Ray Photoelectron Spectrometry.- 20.4.3. Auger-Electron Spectrometry.- 20.4.4. Photo- and Auger-Electron Spectrometer.- 20.5. X-Ray-Excited Optical-Fluorescence Spectrometry.- 20.6. X-Ray Lasers.- 20.7. X-Ray Appearance-Potential Spectrometry.- 21. Electron-Probe Microanalysis.- 21.1. Introduction.- 21.2. Instrumentation.- 21.2.1. General.- 21.2.2. Electron-Optical Systems.- 21.2.3. Other Instrument Systems.- 21.3. Interaction of the Electron Beam and Specimen.- 21.3.1. Interaction Phenomena.- 21.3.1.1. Electron Phenomena.- 21.3.1.2. X-Ray Phenomena.- 21.3.1.3. Cathodoluminescence.- 21.3.1.4. Potential Distribution Pattern.- 21.3.2. Detection.- 21.3.2.1. Electron Detection.- 21.3.2.2. X-Ray, Luminescence, and Potential Detection.- 21.4. Modes of Measurement and Display.- 21.4.1. General.- 21.4.2. Measurement at a Point.- 21.4.3. Measurement along a Line (One-Dimensional Analysis).- 21.4.4. Measurement over a Raster (Two-Dimensional Analysis).- 21.4.5. Measurement Perpendicular to the Specimen Surface (Three-Dimensional Analysis).- 21.4.6. Other Methods of Readout and Display.- 21.4.7. Color Displays.- 21.4.8. Considerations.- 21.5. Specimen Considerations.- 21.6. Quantitative Analysis.- 21.6.1. Principles.- 21.6.2. Intensity Corrections.- 21.7. Performance.- 21.8. Applications.- 21.9. Comparison with X-Ray Fluorescence Spectrometry.- VIII. Appendixes, Bibliography.- Appendixes.- Appendix 1. Wavelengths of the Principal X-Ray Spectral Lines of the Chemical Elements-K Series.- Appendix 2. Wavelengths of the Principal X-Ray Spectral Lines of the Chemical Elements-L Series.- Appendix 3. Wavelengths of the Principal X-Ray Spectral Lines of the Chemical Elements-M Series.- Appendix 4. Photon Energies of the Principal K and L X-Ray Spectral Lines of the Chemical Elements.- Appendix 5. Wavelengths of the K, L, and M X-Ray Absorption Edges of the Chemical Elements.- Appendix 6. K, L, and M X-Ray Excitation Potentials of the Chemical Elements.- Appendix 7A. X-Ray Mass-Absorption Coefficients of the Chemical Elements at 0.1-30 A.- Appendix 7B. X-Ray Mass-Absorption Coefficients of Elements 2-11 (He-Na) at 40-100 A.- Appendix 9. Average Values of the K, L, and M Fluorescent Yields of the Chemical Elements.- Appendix 10. X-Ray Spectrometer Analyzer Crystals and Multilayer Films.- Appendix 11A. Glossary of Frequently Used Notation.- Appendix 11B. Prefixes for Physical Units.- Appendix 12. Periodic Table of the Chemical Elements.- Books.- Periodicals.- General Reviews.- Bibliographies.- Tables of Wavelengths, 2? Angles, and Mass-Absorption Coefficients.- Papers and Reports.