Total reflection X-ray fluorescence analysis and related methods /
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Author / Creator: | Klockenkämper, Reinhold, 1937- author. |
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Edition: | Second edition. |
Imprint: | Hoboken, New Jersey : Wiley, [2015] ©2015 |
Description: | xxvi, 519 pages, 8 pages of plates : illustrations (some color) ; 25 cm. |
Language: | English |
Series: | Chemical analysis ; volume 181 Chemical analysis ; v. 181. |
Subject: | |
Format: | Print Book |
URL for this record: | http://pi.lib.uchicago.edu/1001/cat/bib/10156744 |
Table of Contents:
- Foreword
- Acknowledgments
- List of Acronyms
- List of Physical Units and Subunits
- List of Symbols
- Chapter 1. Fundamentals of X-Ray Fluorescence
- 1.1. A Short History of XRF
- 1.2. The New Variant TXRF
- 1.2.1. Retrospect on its Development
- 1.2.2. Relationship of XRF and TXRF
- 1.3. Nature and Production of X-Rays
- 1.3.1. The Nature of X-Rays
- 1.3.2. X-Ray Tubes as X Ray Sources
- 1.3.2.1. The Line Spectrum
- 1.3.2.2. The Continuous Spectrum
- 1.3.3. Polarization of X-Rays
- 1.3.4. Synchrotron Radiation as X-Ray Source
- 1.3.4.1. Electrons in Fields of Bending Magnets
- 1.3.4.2. Radiation Power of a Single Electron
- 1.3.4.3. Angular and Spectral Distribution of SR
- 1.3.4.4. Comparison with Black-Body Radiation
- 1.4. Attenuation of X-Rays
- 1.4.1. Photoelectric Absorption
- 1.4.2. X-Ray Scatter
- 1.4.3. Total Attenuation
- 1.5. Deflection of X-Rays
- 1.5.1. Reflection and Refraction
- 1.5.2. Diffraction and Bragg's Law
- 1.5.3. Total External Reflection
- 1.5.3.1. Reflectivity
- 1.5.3.2. Penetration Depth
- 1.5.4. Refraction and Dispersion
- References
- Chapter 2. Principles of Total Reflection XRF
- 2.1. Interference of X-Rays
- 2.1.1. Double-Beam Interference
- 2.1.2. Multiple-Beam Interference
- 2.2. X-Ray Standing Wave Fields
- 2.2.1. Standing Waves in Front of a Thick Substrate
- 2.2.2. Standing Wave Fields Within a Thin Layer
- 2.2.3. Standing Waves Within a Multilayer or Crystal
- 2.3. Intensity of Fluorescence Signals
- 2.3.1. Infinitely Thick and Flat Substrates
- 2.3.2. Granular Residues on a Substrate
- 2.3.3. Buried Layers in a Substrate
- 2.3.4. Reflecting Layers on Substrates
- 2.3.5. Periodic Multilayers and Crystals
- 2.4. Formalism For Intensity Calculations
- 2.4.1. A Thick and Flat Substrate
- 2.4.2. A Thin Homogeneous Layer on a Substrate
- 2.4.3. A Stratified Medium of Several Layers
- References
- Chapter 3. Instrumentation for TXRF and GI-XRF
- 3.1. Basic Instrumental Setup
- 3.2. High and Low-Power X-Ray Sources
- 3.2.1. Fine-Focus X-Ray Tubes
- 3.2.2. Rotating Anode Tubes
- 3.2.3. Air-Cooled X-Ray Tubes
- 3.3. Synchrotron Facilities
- 3.3.1. Basic Setup with Bending Magnets
- 3.3.2. Undulators, Wigglers, and FELs
- 3.3.3. Facilities Worldwide
- 3.4. The Beam Adapting Unit
- 3.4.1. Low-Pass Filters
- 3.4.2. Simple Monochromators
- 3.4.3. Double-Crystal Monochromators
- 3.5. Sample Positioning
- 3.5.1. Sample Carriers
- 3.5.2. Fixed Angle Adjustment for TXRF ("Angle Cut")
- 3.5.3. Stepwise-Angle Variation for GI-XRF ("Angle Scan")
- 3.6. Energy-Dispersive Detection of X-Rays
- 3.6.1. The Semiconductor Detector
- 3.6.2. The Silicon Drift Detector
- 3.6.3. Position Sensitive Detectors
- 3.7. Wavelength-Dispersive Detection of X-Rays
- 3.7.1. Dispersing Crystals with Soller Collimators
- 3.7.2. Gas-Filled Detectors
- 3.7.3. Scintillation Detectors
- 3.8. Spectra Registration and Evaluation
- 3.8.1. The Registration Unit
- 3.8.2. Performance Characteristics
- 3.8.2.1. Detector Efficiency
- 3.8.2.2. Spectral Resolution
- 3.8.2.3. Input-Output Yield
- 3.8.2.4. The Escape-Peak Phenomenon
- References
- Chapter 4. Performance of TXRF and GI-XRF Analyses
- 4.1. Preparations for Measurement
- 4.1.1. Cleaning Procedures
- 4.1.2. Preparation of Samples
- 4.1.3. Presentation of a Specimen
- 4.1.3.1. Microliter Sampling by Pipettes
- 4.1.3.2. Nanoliter Droplets by Capillaries
- 4.1.3.3. Picoliter-Sized Droplets by Inkjet Printing
- 4.1.3.4. Microdispensing of Liquids by Triple-Jet Technology
- 4.1.3.5. Solid Matter of Different Kinds
- 4.2. Acquisition of Spectra
- 4.2.1. The Setup for Excitation with X-Ray Tubes
- 4.2.2. Excitation by Synchrotron Radiation
- 4.2.3. Recording the Spectrograms
- 4.2.3.1. Energy-Dispersive Variant
- 4.2.3.2. Wavelength-Dispersive Mode
- 4.3. Qualitative Analysis
- 4.3.1. Shortcomings of Spectra
- 4.3.1.1. Strong Spectral Interferences
- 4.3.1.2. Regard of Sum Peaks
- 4.3.1.3. Dealing with Escape Peaks
- 4.3.2. Unambiguous Element Detection
- 4.3.3. Fingerprint Analysis
- 4.4. Quantitative Micro- and Trace Analyses
- 4.4.1. Prerequisites for Quantification
- 4.4.1.1. Determination of Net Intensities
- 4.4.1.2. Determination of Relative Sensitivities
- 4.4.2. Quantification by Internal Standardization
- 4.4.2.1. Standard Addition for a Single Element
- 4.4.2.2. Multielement Determinations
- 4.4.3. Conditions and Limitations
- 4.4.3.1. Mass and Thickness of Thin Layers
- 4.4.3.2. Residues of Microliter Droplets
- 4.4.3.3. Coherence Length of Radiation
- 4.5. Quantitative Surface and Thin-Layer Analyses by TXRF
- 4.5.1. Distinguishing Between Types of Contamination
- 4.5.1.1. Bulk-Type Impurities
- 4.5.1.2. Particulate Contamination
- 4.5.1.3. Thin-Layer Covering
- 4.5.1.4. Mixture of Contaminations
- 4.5.2. Characterization of Thin Layers by TXRF
- 4.5.2.1. Multifold Repeated Chemical Etching
- 4.5.2.2. Stepwise Repeated Planar Sputter Etching
- 4.6. Quantitative Surface and Thin-Layer Analyses by GI-XRF
- 4.6.1. Recording Angle-Dependent Intensity Profiles
- 4.6.2. Considering the Footprint Effect
- 4.6.3. Regarding the Coherence Length
- 4.6.4. Depth Profiling at Grazing Incidence
- 4.6.5. Including the Surface Roughness
- References
- Chapter 5. Different Fields of Applications
- 5.1. Environmental and Geological Applications
- 5.1.1. Natural Water Samples
- 5.1.2. Airborne Particulates
- 5.1.3. Biomonitoring
- 5.1.4. Geological Samples
- 5.2. Biological and Biochemical Applications
- 5.2.1. Beverages: Water, Tea, Coffee, Must, and Wine
- 5.2.2. Vegetable and Essential Oils
- 5.2.3. Plant Materials and Extracts
- 5.2.4. Unicellular Organisms and Biomolecules
- 5.3. Medical, Clinical, and Pharmaceutical Applications
- 5.3.1. Blood, Plasma, and Serum
- 5.3.2. Urine, Cerebrospinal, and Amniotic Fluid
- 5.3.3. Tissue Samples
- 5.3.3.1. Freeze-Cutting of Organs by a Microtome
- 5.3.3.2. Healthy and Cancerous Tissue Samples
- 5.3.4. Medicines and Remedies
- 5.4. Industrial or Chemical Applications
- 5.4.1. Ultrapure Reagents
- 5.4.2. High-Purity Silicon and Silica
- 5.4.3. Ultrapure Aluminum
- 5.4.4. High-Purity Ceramic Powders
- 5.4.5. Impurities in Nuclear Materials
- 5.4.6. Hydrocarbons and Their Polymers
- 5.4.7. Contamination-Free Wafer Surfaces
- 5.4.7.1. Wafers Controlled by Direct TXRF
- 5.4.7.2. Contaminations Determined by VPD-TXRF
- 5.4.8. Characterization of Nanostructured Samples
- 5.4.8.1. Shallow Layers by Sputter Etching and TXRF
- 5.4.8.2. Thin-Layer Structures by Direct GT-XRF
- 5.4.8.3. Nanoparticles by TXRF and GI-XRF
- 5.5. Art Historical and Forensic Applications
- 5.5.1. Pigments, Inks, and Varnishes
- 5.5.2. Metals and Alloys
- 5.5.3. Textile Fibers and Glass Splinters
- 5.5.4. Drug Abuse and Poisoning
- References
- Chapter 6. Efficiency and Evaluation
- 6.1. Analytical Considerations
- 6.1.1. General Costs of Installation and Upkeep
- 6.1.2. Detection Power for Elements
- 6.1.3. Reliability of Determinations
- 6.1.4. The Great Variety of Suitable Samples
- 6.1.5. Round-Robin Tests
- 6.2. Utility and Competitiveness of TXRF and GI-XRF
- 6.2.1. Advantages and Limitations
- 6.2.2. Comparison of TXRF with Competitors
- 6.2.3. GI-XRF and Competing Methods
- 6.3. Perception and Propagation of TXRF Methods
- 6.3.1. Commercially Available Instruments
- 6.3.2. Support by the International Atomic Energy Agency
- 6.3.3. Worldwide Distribution of TXRF and Related Methods
- 6.3.4. Standardization by ISO and DIN
- 6.3.5. International Cooperation and Activity
- References
- Chapter 7. Trends and Future Prospects
- 7.1. Instrumental Developments
- 7.1.1. Excitation by Synchrotron Radiation
- 7.1.2. New Variants of X-Ray Sources
- 7.1.3. Capillaries and Waveguides for Beam Adapting
- 7.1.4. New Types of X-Ray Detectors
- 7.2. Methodical Developments
- 7.2.1. Detection of Light Elements
- 7.2.2. Ablation and Deposition Techniques
- 7.2.3. Grazing Exit X-Ray Fluorescence
- 7.2.4. Reference-Free Quantification
- 7.2.5. Time-Resolved In Situ Analysis
- 7.3. Future Prospects by Combinations
- 7.3.1. Combination with X-Ray Reflectometry
- 7.3.2. EXAFS and Total Reflection Geometry
- 7.3.3. Combination with XANES or NEXAFS
- 7.3.4. X-Ray Diffractometry at Total Reflection
- 7.3.5. Total Reflection and X-Ray Photoelectron Spectrometry
- References
- Index