X-Ray Fluorescence Spectroscopy for Laboratory Applications

Preface xvii
List of Abbreviations and Symbols xix
About the Authors xxiii

1 Introduction 1

2 Principles of X-ray Spectrometry 7
2.1 Analytical Performance 7
2.2 X-ray Radiation and Their Interaction 11
2.3 The Development of X-ray Spectrometry 21
2.4 Carrying Out an Analysis 26

3 Sample Preparation 31
3.1 Objectives of Sample Preparation 31
3.2 Preparation Techniques 32
3.3 Preparation of Compact and Homogeneous Materials 39
3.4 Small Parts Materials 41
3.5 Liquid Samples 55
3.6 Biological Materials 58
3.7 Small Particles, Dust, and Aerosols 59

4 XRF Instrument Types 61
4.1 General Design of an X-ray Spectrometer 61
4.2 Comparison of Wavelength- and Energy-Dispersive X-Ray Spectrometers 63
4.2.5 Radiation Flux 75
4.3 Type of Instruments 80
4.4 Commercially Available Instrument Types 98

5 Measurement and Evaluation of X-ray Spectra 99
5.1 Information Content of the Spectra 99
5.2 Procedural Steps to Execute a Measurement 101
5.3 Selecting the Measurement Conditions 102
5.4 Determination of Peak Intensity 112
5.5 Quanti¿cation Models 117
5.6 Characterization of Layered Materials 133
5.7 Chemometric Methods for Material Characterization 140
5.8 Creation of an Application 143

6 Analytical Errors 149
6.1 General Considerations 149
6.2 Types of Errors 156
6.3 Accounting for Systematic Errors 159
6.4 Recording of Error Information 164

7 Other Element Analytical Methods 167
7.1 Overview 167
7.2 Atomic Absorption Spectrometry (AAS) 168
7.3 Optical Emission Spectrometry 169
7.4 Mass Spectrometry (MS) 172
7.5 X-Ray Spectrometry by Particle Excitation (SEM-EDS, PIXE) 173
7.6 Comparison of Methods 175

8 Radiation Protection 177
8.1 Basic Principles 177
8.2 E¿ects of Ionizing Radiation on Human Tissue 178
8.3 Natural Radiation Exposure 179
8.4 Radiation Protection Regulations 181
8.4.1 Legal Regulations 181

9 Analysis of Homogeneous Solid Samples 183
9.1 Iron Alloys 183
9.2 Ni?Fe?Co Alloys 188
9.3 Copper Alloys 189
9.4 Aluminum Alloys 191
9.5 Special Metals 192
9.5.1 Refractories 192
9.6 Precious Metals 195
9.7 Glass Material 199
9.8 Polymers 203
9.9 Abrasion Analysis 209

10 Analysis of Powder Samples 213
10.1 Geological Samples 213
10.2 Ores 216
10.3 Soils and Sewage Sludges 221
10.4 Quartz Sand 223
10.5 Cement 223
10.6 Coal and Coke 227
10.7 Ferroalloys 230
10.8 Slags 235
10.9 Ceramics and Refractory Materials 237
10.10 Dusts 239
10.11 Food 242
10.12 Pharmaceuticals 245
10.13 Secondary Fuels 246

11 Analysis of Liquids 253
11.1 Multielement Analysis of Liquids 254
11.2 Fuels and Oils 255
11.3 Trace Analysis in Liquids 261
11.4 Special Preparation Techniques for Liquid Samples 263

12 Trace Analysis Using Total Re¿ection X-Ray Fluorescence 267
12.1 Special Features of TXRF 267
12.2 Sample Preparation for TXRF 269
12.3 Evaluation of the Spectra 271
12.4 Typical Applications of the TXRF 274

13 Nonhomogeneous Samples 287
13.1 Measurement Modes 287
13.2 Instrument Requirements 288
13.3 Data Evaluation 290

14 Coating Analysis 291
14.1 Analytical Task 291
14.2 Sample Handling 292
14.3 Measurement Technology 293
14.4 The Analysis Examples of Coated Samples 294

15 Spot Analyses 313
15.1 Particle Analyses 313
15.2 Identi¿cation of Inclusions 318
15.3 Material Identi¿cation with Handheld Instruments 318
15.4 Determination of Toxic Elements in Consumer Products: RoHS Monitoring 324
15.5 Toxic Elements in Toys: Toys Standard 328

16 Analysis of Element Distributions 331
16.1 General Remarks 331
16.2 Measurement Conditions 332
16.3 Geology 333
16.4 Electronics 342
16.5 Archeometric Investigations 344
16.6 Homogeneity Tests 350

17 Special Applications of the XRF 355
17.2 Chemometric Spectral Evaluation 358
17.3 High-Resolution Spectroscopy for Speciation Analysis 361

18 Process Control and Automation 367
18.1 General Objectives 367
18.2 O¿-Line and At-Line Analysis 369
18.3 In-Line and On-Line Analysis 376
19 Quality Management and Validation 379
19.1 Motivation 379
19.2 Validation 380

Appendix A Tables 387
Appendix B Important Inf