Atomic and Nuclear Analytical Methods
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1 H.R. Verma Atomic and Nuclear Analytical Methods XRF, Mössbauer, XPS, NAA and Ion-Beam Spectroscopic Techniques With 128 Figures and 24 Tables Springer
2 Contents 1 X-ray Fluorescence (XRF) and Particle-Induced X-ray Emission (PIXE) Introduction Principle of XRF and PIXE Techniques Theory and Concept Spectral Series, The Moseley Law Line Intensities and Fluorescence Yield Critical Excitation Energies of the Exciting Radiation/Particles Instrumentation/Experimentation Modes of Excitation for XRF Analysis X-ray Detection and Analysis in XRF Source of Excitation and X-ray Detection in PIXE Analysis Some Other Aspects Connected with PIXE Analysis Qualitative and Quantitative Analysis Thick vs. Thin Samples Formalism for Thin-Target XRF Formalism for Thick-Target XRF Formalism for Thin-Target FIXE Formalism for Thick-Target PIXE Counting Statistics and Minimum Detection Limit Sources of Background Contribution of Exciter Source to Signal Background Contribution of Scattering Geometry to Signal Background Contribution of Detection System to Signal Background Methods for Improving Detection Limits Computer Analysis of X-Ray Spectra 70
3 X Contents 1.11 Some Other Topics Related to PIXE Analysis Depth Profiling of Materials by PIXE Proton Microprobes Theories of X-Ray Emission by Charged Particles Applications of XRF and PIXE Techniques In Biological Sciences In Criminology In Material Science Pollution Analysis For Archaeological Samples For Chemical Analysis of Samples For Analysis of Mineral Samples Comparison Between EDXRF and WDXRF Techniques Resolution Simultaneity Spectral Overlaps Background Excitation Efficiency Comparison Between XRF and PIXE Techniques Conclusion 90 2 Rutherford Backscattering Spectroscopy Introduction Scattering Fundamentals Impact Parameter, Scattering Angle, and Distance of Closest Approach Kinematic Factor Stopping Power, Energy Loss, Range, and Straggling Energy of Particles Backscattered from Thin and Thick Targets Stopping Cross-Section Rutherford Scattering Cross-Section Principle of Rutherford Backscattering Spectroscopy Fundamentals of the RBS Technique and its Characteristics Deviations from Rutherford Formula Non-Rutherford Cross-Sections Shielded Rutherford Cross-Sections Instrumentation/Experimental Accelerator, Beam Transport System, and Scattering Chamber Particle Detectors RBS Spectra from Thin and Thick Layers RBS Spectrum from a Thin Layers RBS Spectrum from Thick Layers 121
4 Contents XI 2.8 Spectrum Analysis/Simulation Heavy Ion Backscattering Spectrometry High-Resolution RBS Medium Energy Ion Scattering Channeling Rutherford Scattering Using Forward Angles Applications of RBS Limitation of the RBS Technique Elastic Recoil Detection Introduction Fundamentals of the ERDA Technique Kinematic Factor Scattering Cross-Sections and Depth Resolution in ERD Stopping Power and Straggling Principle and Characteristics of ERDA Experimental ERDA Using E-Detection (Conventional Set-Up) ERDA with Particle Identification and Depth Resolution Heavy Ion ERDA Data Analysis Advantages and Limitations of ERDA Mössbauer Spectroscopy (MS) Introduction Concept and Theory Nuclear Resonance Fluorescence Nuclear Physics of 57Fe Lamb Mössbauer Factor (Recoil-Free Fraction) Some Other Mössbauer Isotopes and their y-transitions Characteristic Parameters Obtainable Through Mössbauer Spectroscopy Experimental Set-Up A Basic Mössbauer Spectrometer Set-Up Advances in Experimental Set-Up/Method of Analysis Evaluation of Mössbauer Spectra Conversion Electron Mössbauer Spectroscopy Applications Chemical Analysis Nondestructive Testing and Surface Studies Investigation of New Materials for Industrial Applications 207
5 XII Contents Characterization of Nanostructured Materials Testing of Reactor Steel In Mars Exploration Study of Actinides Study of Biological Materials Investigation of Lattice Dynamits Using the Rayleigh Scattering of Mössbauer y-rays X-Ray Photoelectron Spectroscopy Introduction Principle and Characteristics of XPS Instrumentation/Experimental Commonly Used X-ray Sources for XPS Analysis Photoelectron Analyzers/Detectors Experimental Workstation Data Acquisition and Analysis Principle Photoelectron Lines for a Few Elements Salient Features of XPS and a Few Practical Examples Applications of XPS Microanalysis of the Surfaces of Metals and Alloys Study of Mineral Surfaces Study of Polymers Study of Material Used for Medical Purpose For Surface Characterization of Coal Ash Surface Study of Cements and Concretes Study of High Energy Resolution Soft X-rays Core Level Photoemission in the Study of Basic Atomic Physics Advantages and Limitations of XPS Neutron Activation Analysis Introduction Principle Prompt vs. Delayed NAA Epithermal and Fast Neutron Activation Analysis Experimental Neutron Sources A Few Radioisotopes Formed Through (n, y) Reaction (Used for Elemental Identification) and their Half-Lives Scintillation and Semiconductor y-ray Detectors 'y-ray Spectrometer Quantitative Analysis Using NAA Absolute Method for a Single Element Comparison Method Simulation: MCNP Code 260
6 Contents XIII 6.5 Sensitivities Available by NAA Applications of NAA In Archaeology In Biochemistry In Ecological Monitoring of Environment In Microanalysis of Biological Materials In Forensic Investigations In Geological Science In Material Science (Detection of Components of Metals, Semiconductors, and Alloys) In Soil Science, Agriculture, and Building Materials For Analysis of Food Items and Ayurvedic Medicinal Materials Detection of Explosives, Fissile Materials, and Drugs Advantages and Limitations of NAA Advantages of NAA Limitations of NAA Nuclear Reaction Analysis and Particle-Induced Gamma-Ray Emission Introduction Principle of NRA Reaction Kinematics for NRA Examples of Some Important Reactions Particle-Induced y-emission Analysis Experimental Methods Detection Limit/Sensitivity Applications of NRA For Material Analysis For Depth Profiling Studies For Tracer Studies and for the Study of Medical Samples For the Study of Archaeological Samples Applications of PIGE For Material Analysis For the Study of Medical Samples For the Study of Archaeological Sample For the Study of Aerosol Samples For the Study of Soil, Concrete, Rocks, and Geochemical Samples Common Particle Particle Nuclear Reactions Proton-Induced Reactions Deuteron-Induced Reactions He-, 4He-Induced Reactions Some Important Reactions Used for NRA Analysis Some Important Reactions Used for PIGE Analysis 293
7 XIV Contents 8 Accelerator Mass Spectrometry (AMS) Introduction Principle Experimental AMS Using Low-Energy Accelerators Sample Preparation for AMS Time-of-Flight Mass Spectrometry (TOF-MS) Detection Limits of Particles Analyzed by AMS Applications of AMS In the Field of Archeology In the Field of Earth Science For Study of Pollution In the Field of Biomedicine In the Field of Hydrology In Material Analysis In the Field of Food Chemistry For Study of Nutrients In the Field of Geological Science For Study of Ice-Cores Use of Various Isotopes for Important AMS Studies Use of 10Be Use of 14 C Use of 26A Use of 36C Use of 41 Ca Use of 59Ni AMS of Molecular Ions Advantages and Limitations of AMS 319 A Appendix 323 A.1 Some Useful Data Tables 323 B Appendix 333 B.1 Relation of Energies, Scattering Angles, and Rutherford Scattering Cross-Sections in the Center-of-Mass System and Laboratory System 333 C Appendix 339 References 341 Index 365
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