Reinhold Klockenkämper, Alex von Bohlen

Total-Reflection X-Ray Fluorescence Analysis and Related Methods (eBook, PDF)

• Format: PDF

Produktbeschreibung

Explores the uses of TXRF in micro- and trace analysis, and in surface- and near-surface-layer analysis * Pinpoints new applications of TRXF in different fields of biology, biomonitoring, material and life sciences, medicine, toxicology, forensics, art history, and archaeometry * Updated and detailed sections on sample preparation taking into account nano- and picoliter techniques * Offers helpful tips on performing analyses, including sample preparations, and spectra recording and interpretation * Includes some 700 references for further study

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Produktdetails

• Verlag: John Wiley & Sons
• Seitenzahl: 552
• Erscheinungstermin: 10. Dezember 2014
• Englisch
• ISBN-13: 9781118985878
• Artikelnr.: 42009716

Autorenporträt

Reinhold Klockenkämper is physicist and was head of the Physical Analysis Research Group at ISAS in Dortmund, Germany. Furthermore, he was Associate Lecturer at the University of Applied Sciences in Dortmund. His experience in X-ray spectral analysis spans four decades and he published over 100 scientific papers and several book articles. He was member of three Editorial Advisory Boards of international journals for many years. In 1988 and 1996 he organized the 2nd and the 6th conference on TXRF in Dortmund. In 1996 he published the first edition of this monograph on TXRF. Professor Klockenkämper retired in 2002, but is currently working as guest scientist at ISAS. Alex von Bohlen is engineer and senior scientist at the Leibniz-Institut für Analytische Wissenschaften -ISAS- e.V. in Dortmund. He is head of the X-ray laboratories and of the scanning electron and optical microscopy facilities. In addition, he is responsible for the beamline 2 at DELTA, Center for Synchrotron Radiation at the Technical University of Dortmund. Dr. von Bohlen has been working in the field of TXRF since more than 25 years, has published more than 120 articles, mostly dedicated to TXRF, and is member of two Editorial Advisary Boards. In 2011 he organized the 14th conference on TXRF in Dortmund.

Inhaltsangabe

FOREWORD xiii ACKNOWLEDGMENTS xv LIST OF ACRONYMS xvii LIST OF PHYSICAL
UNITS AND SUBUNITS xxii LIST OF SYMBOLS xxiii CHAPTER 1 FUNDAMENTALS OF
X-RAY FLUORESCENCE 1 1.1 A Short History of XRF 2 1.2 The New Variant TXRF
8 1.2.1 Retrospect on its Development 8 1.2.2 Relationship of XRF and TXRF
13 1.3 Nature and Production of X-Rays 15 1.3.1 The Nature of X-Rays 15
1.3.2 X-Ray Tubes as X-Ray Sources 17 1.3.2.1 The Line Spectrum 19 1.3.2.2
The Continuous Spectrum 27 1.3.3 Polarization of X-Rays 29 1.3.4
Synchrotron Radiation as X-Ray Source 30 1.3.4.1 Electrons in Fields of
Bending Magnets 32 1.3.4.2 Radiation Power of a Single Electron 35 1.3.4.3
Angular and Spectral Distribution of SR 36 1.3.4.4 Comparison with
Black-Body Radiation 42 1.4 Attenuation of X-Rays 44 1.4.1 Photoelectric
Absorption 46 1.4.2 X-Ray Scatter 49 1.4.3 Total Attenuation 51 1.5
Deflection of X-Rays 53 1.5.1 Reflection and Refraction 53 1.5.2
Diffraction and Bragg's Law 59 1.5.3 Total External Reflection 62 1.5.3.1
Reflectivity 66 1.5.3.2 Penetration Depth 67 1.5.4 Refraction and
Dispersion 71 References 74 CHAPTER 2 PRINCIPLES OF TOTAL REFLECTION XRF 79
2.1 Interference of X-Rays 80 2.1.1 Double-Beam Interference 80 2.1.2
Multiple-Beam Interference 84 2.2 X-Ray Standing Wave Fields 88 2.2.1
Standing Waves in Front of a Thick Substrate 88 2.2.2 Standing Wave Fields
Within a Thin Layer 94 2.2.3 Standing Waves Within a Multilayer or Crystal
100 2.3 Intensity of Fluorescence Signals 100 2.3.1 Infinitely Thick and
Flat Substrates 102 2.3.2 Granular Residues on a Substrate 104 2.3.3 Buried
Layers in a Substrate 106 2.3.4 Reflecting Layers on Substrates 108 2.3.5
Periodic Multilayers and Crystals 110 2.4 Formalism For Intensity
Calculations 112 2.4.1 A Thick and Flat Substrate 113 2.4.2 A Thin
Homogeneous Layer on a Substrate 116 2.4.3 A Stratified Medium of Several
Layers 120 References 123 CHAPTER 3 INSTRUMENTATION FOR TXRF AND GI-XRF 126
3.1 Basic Instrumental Setup 128 3.2 High and Low-Power X-Ray Sources 130
3.2.1 Fine-Focus X-Ray Tubes 131 3.2.2 Rotating Anode Tubes 132 3.2.3
Air-Cooled X-Ray Tubes 133 3.3 Synchrotron Facilities 134 3.3.1 Basic Setup
with Bending Magnets 136 3.3.2 Undulators, Wigglers, and FELs 137 3.3.3
Facilities Worldwide 139 3.4 The Beam Adapting Unit 150 3.4.1 Low-Pass
Filters 150 3.4.2 Simple Monochromators 155 3.4.3 Double-Crystal
Monochromators 157 3.5 Sample Positioning 160 3.5.1 Sample Carriers 161
3.5.2 Fixed Angle Adjustment for TXRF ("Angle Cut") 162 3.5.3
Stepwise-Angle Variation for GI-XRF ("Angle Scan") 162 3.6
Energy-Dispersive Detection of X-Rays 164 3.6.1 The Semiconductor Detector
165 3.6.2 The Silicon Drift Detector 167 3.6.3 Position Sensitive Detectors
169 3.7 Wavelength-Dispersive Detection of X-Rays 173 3.7.1 Dispersing
Crystals with Soller Collimators 176 3.7.2 Gas-Filled Detectors 178 3.7.3
Scintillation Detectors 182 3.8 Spectra Registration and Evaluation 183
3.8.1 The Registration Unit 183 3.8.2 Performance Characteristics 185
3.8.2.1 Detector Efficiency 185 3.8.2.2 Spectral Resolution 188 3.8.2.3
Input-Output Yield 194 3.8.2.4 The Escape-Peak Phenomenon 197 References
200 CHAPTER 4 PERFORMANCE OF TXRF AND GI-XRF ANALYSES 205 4.1 Preparations
for Measurement 207 4.1.1 Cleaning Procedures 207 4.1.2 Preparation of
Samples 211 4.1.3 Presentation of a Specimen 215 4.1.3.1 Microliter
Sampling by Pipettes 216 4.1.3.2 Nanoliter Droplets by Capillaries 217
4.1.3.3 Picoliter-Sized Droplets by Inkjet Printing 218 4.1.3.4
Microdispensing of Liquids by Triple-Jet Technology 220 4.1.3.5 Solid
Matter of Different Kinds 220 4.2 Acquisition of Spectra 222 4.2.1 The
Setup for Excitation with X-Ray Tubes 222 4.2.2 Excitation by Synchrotron
Radiation 225 4.2.3 Recording the Spectrograms 226 4.2.3.1
Energy-Dispersive Variant 227 4.2.3.2 Wavelength-Dispersive Mode 227 4.3
Qualitative Analysis 228 4.3.1 Shortcomings of Spectra 228 4.3.1.1 Strong
Spectral Interferences 229 4.3.1.2 Regard of Sum Peaks 235 4.3.1.3 Dealing
with Escape Peaks 235 4.3.2 Unambiguous Element Detection 236 4.3.3
Fingerprint Analysis 237 4.4 Quantitative Micro- and Trace Analyses 238
4.4.1 Prerequisites for Quantification 240 4.4.1.1 Determination of Net
Intensities 240 4.4.1.2 Determination of Relative Sensitivities 241 4.4.2
Quantification by Internal Standardization 244 4.4.2.1 Standard Addition
for a Single Element 245 4.4.2.2 Multielement Determinations 246 4.4.3
Conditions and Limitations 248 4.4.3.1 Mass and Thickness of Thin Layers
249 4.4.3.2 Residues of Microliter Droplets 251 4.4.3.3 Coherence Length of
Radiation 252 4.5 Quantitative Surface and Thin-Layer Analyses by TXRF 257
4.5.1 Distinguishing Between Types of Contamination 257 4.5.1.1 Bulk-Type
Impurities 257 4.5.1.2 Particulate Contamination 258 4.5.1.3 Thin-Layer
Covering 259 4.5.1.4 Mixture of Contaminations 259 4.5.2 Characterization
of Thin Layers by TXRF 262 4.5.2.1 Multifold Repeated Chemical Etching 262
4.5.2.2 Stepwise Repeated Planar Sputter Etching 264 4.6 Quantitative
Surface and Thin-Layer Analyses by GI-XRF 267 4.6.1 Recording
Angle-Dependent Intensity Profiles 268 4.6.2 Considering the Footprint
Effect 270 4.6.3 Regarding the Coherence Length 272 4.6.4 Depth Profiling
at Grazing Incidence 274 4.6.5 Including the Surface Roughness 283
References 284 CHAPTER 5 DIFFERENT FIELDS OF APPLICATIONS 291 5.1
Environmental and Geological Applications 292 5.1.1 Natural Water Samples
292 5.1.2 Airborne Particulates 297 5.1.3 Biomonitoring 302 5.1.4
Geological Samples 306 5.2 Biological and Biochemical Applications 307
5.2.1 Beverages: Water, Tea, Coffee, Must, and Wine 308 5.2.2 Vegetable and
Essential Oils 312 5.2.3 Plant Materials and Extracts 312 5.2.4 Unicellular
Organisms and Biomolecules 315 5.3 Medical, Clinical, and Pharmaceutical
Applications 317 5.3.1 Blood, Plasma, and Serum 317 5.3.2 Urine,
Cerebrospinal, and Amniotic Fluid 320 5.3.3 Tissue Samples 322 5.3.3.1
Freeze-Cutting of Organs by a Microtome 322 5.3.3.2 Healthy and Cancerous
Tissue Samples 324 5.3.4 Medicines and Remedies 327 5.4 Industrial or
Chemical Applications 329 5.4.1 Ultrapure Reagents 330 5.4.2 High-Purity
Silicon and Silica 331 5.4.3 Ultrapure Aluminum 332 5.4.4 High-Purity
Ceramic Powders 334 5.4.5 Impurities in Nuclear Materials 336 5.4.6
Hydrocarbons and Their Polymers 336 5.4.7 Contamination-Free Wafer Surfaces
338 5.4.7.1 Wafers Controlled by Direct TXRF 340 5.4.7.2 Contaminations
Determined by VPD-TXRF 342 5.4.8 Characterization of Nanostructured Samples
346 5.4.8.1 Shallow Layers by Sputter Etching and TXRF 346 5.4.8.2
Thin-Layer Structures by Direct GI-XRF 347 5.4.8.3 Nanoparticles by TXRF
and GI-XRF 354 5.5 Art Historical and Forensic Applications 357 5.5.1
Pigments, Inks, and Varnishes 357 5.5.2 Metals and Alloys 361 5.5.3 Textile
Fibers and Glass Splinters 363 5.5.4 Drug Abuse and Poisoning 365
References 367 CHAPTER 6 EFFICIENCY AND EVALUATION 383 6.1 Analytical
Considerations 384 6.1.1 General Costs of Installation and Upkeep 384 6.1.2
Detection Power for Elements 385 6.1.3 Reliability of Determinations 388
6.1.4 The Great Variety of Suitable Samples 391 6.1.5 Round-Robin Tests 393
6.2 Utility and Competitiveness of TXRF and GI-XRF 397 6.2.1 Advantages and
Limitations 398 6.2.2 Comparison of TXRF with Competitors 400 6.2.3 GI-XRF
and Competing Methods 409 6.3 Perception and Propagation of TXRF Methods
410 6.3.1 Commercially Available Instruments 410 6.3.2 Support by the
International Atomic Energy Agency 413 6.3.3 Worldwide Distribution of TXRF
and Related Methods 413 6.3.4 Standardization by ISO and DIN 417 6.3.5
International Cooperation and Activity 420 References 424 CHAPTER 7 TRENDS
AND FUTURE PROSPECTS 433 7.1 Instrumental Developments 434 7.1.1 Excitation
by Synchrotron Radiation 434 7.1.2 New Variants of X-Ray Sources 436 7.1.3
Capillaries and Waveguides for Beam Adapting 438 7.1.4 New Types of X-Ray
Detectors 442 7.2 Methodical Developments 445 7.2.1 Detection of Light
Elements 445 7.2.2 Ablation and Deposition Techniques 449 7.2.3 Grazing
Exit X-Ray Fluorescence 452 7.2.4 Reference-Free Quantification 459 7.2.5
Time-Resolved In Situ Analysis 462 7.3 Future Prospects by Combinations 463
7.3.1 Combination with X-Ray Reflectometry 464 7.3.2 EXAFS and Total
Reflection Geometry 466 7.3.3 Combination with XANES or NEXAFS 468 7.3.4
X-Ray Diffractometry at Total Reflection 480 7.3.5 Total Reflection and
X-Ray Photoelectron Spectrometry 486 References 491 INDEX 501