X-Ray Fluorescence Spectroscopy for Laboratory Applications

; Joerg Flock ; Michael Haller

Provides comprehensive coverage on using X-ray fluorescence for laboratory applications


This 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. Les mer
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Om boka

Provides comprehensive coverage on using X-ray fluorescence for laboratory applications


This 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 results



X-Ray Fluorescence Spectroscopy for Laboratory Applications appeals to analytical chemists, analytical laboratories, materials scientists, environmental chemists, chemical engineers, biotechnologists, and pharma engineers.

Fakta

Innholdsfortegnelse

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 Information 419


B.1 Coordinates of Main Manufacturers of Instruments and Preparation Tools 419


B.2 Main Suppliers of Standard Materials 422


B.3 Important Websites 425


B.4 Laws and Acts, Which Are Important for X-Ray Fluorescence 427





References 435





Index 453


Om forfatteren

Michael Haschke, PhD, has been working in the product management of various companies for more than 35 years where he was responsible for the development and introduction to market of new x-ray fluorescence techniques, mainly in the field of energy-dissipative spectroscopy.





Joerg Flock, PhD, is Head of the Central Laboratory of ThyssenKrupp Stahl AG and well-versed with different analytical techniques, in particular with x-ray fluorescence spectroscopy. He has extensive practical experience in using this technique for the analysis of samples with different qualities and the interpretation of the acquired results.





Michael Haller has been using X-rays as an analytical tool for over thirty years, first in X-ray crystallography, then later in the development and application of polycapillary X-ray optics. Further he has developed new applications for coating thickness instruments. In 2018 he became co-owner of CrossRoads Scientific, a company specializing in the development of analytical X-ray software.