X-Ray Fluorescence Spectroscopy for Laboratory Applications

Provides comprehensive coverage on using X-ray fluorescence for laboratory applicationsThis book focuses on the practical aspects of X-ray fluorescence (XRF) spectroscopy and discusses the requirements for a successful sample analysis, such as sample preparation, measurement techniques and calibration, as well as the quality of the analysis results.X-Ray Fluorescence Spectroscopy for Laboratory Applications begins with a short overview of the physical fundamentals of the generation of X-rays and their interaction with the sample material, followed by a presentation of the different methods of sample preparation in dependence on the quality of the source material and the objective of the measurement. After a short description of the different available equipment types and their respective performance, the book provides in-depth information on the choice of the optimal measurement conditions and the processing of the measurement results. It covers instrument types for XRF; acquisition and evaluation of X-Ray spectra; analytical errors; analysis of homogeneous materials, powders, and liquids; special applications of XRF; process control and automation.* An important resource for the analytical chemist, providing concrete guidelines and support for everyday analyses* Focuses on daily laboratory work with commercially available devices* Offers a unique compilation of knowledge and best practices from equipment manufacturers and users* Covers the entire work process: sample preparation, the actual measurement, data processing, assessment of uncertainty, and accuracy of the obtained resultsX-Ray Fluorescence Spectroscopy for Laboratory Applications appeals to analytical chemists, analytical laboratories, materials scientists, environmental chemists, chemical engineers, biotechnologists, and pharma engineers.

Preface xviiList of Abbreviations and Symbols xixAbout the Authors xxiii1 Introduction 12 Principles of X-ray Spectrometry 72.1 Analytical Performance 72.2 X-ray Radiation and Their Interaction 112.3 The Development of X-ray Spectrometry 212.4 Carrying Out an Analysis 263 Sample Preparation 313.1 Objectives of Sample Preparation 313.2 Preparation Techniques 323.3 Preparation of Compact and Homogeneous Materials 393.4 Small Parts Materials 413.5 Liquid Samples 553.6 Biological Materials 583.7 Small Particles, Dust, and Aerosols 594 XRF Instrument Types 614.1 General Design of an X-ray Spectrometer 614.2 Comparison of Wavelength- and Energy-Dispersive X-Ray Spectrometers 634.2.5 Radiation Flux 754.3 Type of Instruments 804.4 Commercially Available Instrument Types 985 Measurement and Evaluation of X-ray Spectra 995.1 Information Content of the Spectra 995.2 Procedural Steps to Execute a Measurement 1015.3 Selecting the Measurement Conditions 1025.4 Determination of Peak Intensity 1125.5 Quanti¿cation Models 1175.6 Characterization of Layered Materials 1335.7 Chemometric Methods for Material Characterization 1405.8 Creation of an Application 1436 Analytical Errors 1496.1 General Considerations 1496.2 Types of Errors 1566.3 Accounting for Systematic Errors 1596.4 Recording of Error Information 1647 Other Element Analytical Methods 1677.1 Overview 1677.2 Atomic Absorption Spectrometry (AAS) 1687.3 Optical Emission Spectrometry 1697.4 Mass Spectrometry (MS) 1727.5 X-Ray Spectrometry by Particle Excitation (SEM-EDS, PIXE) 1737.6 Comparison of Methods 1758 Radiation Protection 1778.1 Basic Principles 1778.2 E¿ects of Ionizing Radiation on Human Tissue 1788.3 Natural Radiation Exposure 1798.4 Radiation Protection Regulations 1818.4.1 Legal Regulations 1819 Analysis of Homogeneous Solid Samples 1839.1 Iron Alloys 1839.2 Ni?Fe?Co Alloys 1889.3 Copper Alloys 1899.4 Aluminum Alloys 1919.5 Special Metals 1929.5.1 Refractories 1929.6 Precious Metals 1959.7 Glass Material 1999.8 Polymers 2039.9 Abrasion Analysis 20910 Analysis of Powder Samples 21310.1 Geological Samples 21310.2 Ores 21610.3 Soils and Sewage Sludges 22110.4 Quartz Sand 22310.5 Cement 22310.6 Coal and Coke 22710.7 Ferroalloys 23010.8 Slags 23510.9 Ceramics and Refractory Materials 23710.10 Dusts 23910.11 Food 24210.12 Pharmaceuticals 24510.13 Secondary Fuels 24611 Analysis of Liquids 25311.1 Multielement Analysis of Liquids 25411.2 Fuels and Oils 25511.3 Trace Analysis in Liquids 26111.4 Special Preparation Techniques for Liquid Samples 26312 Trace Analysis Using Total Re¿ection X-Ray Fluorescence 26712.1 Special Features of TXRF 26712.2 Sample Preparation for TXRF 26912.3 Evaluation of the Spectra 27112.4 Typical Applications of the TXRF 27413 Nonhomogeneous Samples 28713.1 Measurement Modes 28713.2 Instrument Requirements 28813.3 Data Evaluation 29014 Coating Analysis 29114.1 Analytical Task 29114.2 Sample Handling 29214.3 Measurement Technology 29314.4 The Analysis Examples of Coated Samples 29415 Spot Analyses 31315.1 Particle Analyses 31315.2 Identi¿cation of Inclusions 31815.3 Material Identi¿cation with Handheld Instruments 31815.4 Determination of Toxic Elements in Consumer Products: RoHS Monitoring 32415.5 Toxic Elements in Toys: Toys Standard 32816 Analysis of Element Distributions 33116.1 General Remarks 33116.2 Measurement Conditions 33216.3 Geology 33316.4 Electronics 34216.5 Archeometric Investigations 34416.6 Homogeneity Tests 35017 Special Applications of the XRF 35517.2 Chemometric Spectral Evaluation 35817.3 High-Resolution Spectroscopy for Speciation Analysis 36118 Process Control and Automation 36718.1 General Objectives 36718.2 O¿-Line and At-Line Analysis 36918.3 In-Line and On-Line Analysis 37619 Quality Management and Validation 37919.1 Motivation 37919.2 Validation 380Appendix A Tables 387Appendix B Important Inf