The Analysis of Nuclear Materials and Their Environments (eBook)

Claude Degueldre is a Professor of Nuclear Engineering at the Department of Engineering of the Lancaster University, UK. His research deals with the analysis of nuclear materials and their environments. He used to teach a course on the behavior of radionuclides in the environment at the Institute for Environmental Science, University of Geneva, Switzerland. He also worked for 30 years in nuclear sciences at the Paul Scherrer Institute, Villigen, Switzerland, focusing on research in the field of the nuclear fuel cycle.

Foreword 5
Preface 7
Acknowledgements 10
Contents 11
Abbreviations 14
Materials 18
System and Organization 18
Units 19
Constants 19
Parameters 19
1 Background: Nuclear Materials and Their Analysis Needs 22
1.1 Materials 22
1.2 Nuclear Materials 26
1.2.1 Generation 0 Reactors Materials 27
1.2.2 From Generation I to II Reactor Materials 28
1.2.3 Generation III Reactor Materials 30
1.2.4 Generation IV Reactor Materials 31
1.2.5 Materials from Generation V Reactors and Accelerators 33
1.2.6 Military Nuclear Materials 34
1.2.7 Nuclear Waste Management 37
1.2.8 Contaminated Materials 39
1.3 Analysis Needs and Limitations 40
1.3.1 Required Analyses and Analysis Requirement 40
1.3.2 Analytical Limitations 41
1.3.3 Analysis Modes and Combinations 43
References 44
2 Sampling, Handling, Treatment and Separation 46
2.1 Sample Collection and Analysis Mode 46
2.1.1 Sample Selection and Collection 46
2.1.2 Sampling from Analysis Mode 48
2.2 Sub-sampling 49
2.2.1 Fluid Samples 50
2.2.2 Solid Samples 50
2.3 Reference Materials and Calibration 53
2.3.1 Reference Materials 53
2.3.2 Calibration with Internal or External Standards 54
References 54
3 Characterization Using Passive or Interactive Techniques 56
3.1 Material Characterization by Field-Free Passive Techniques 59
3.1.1 Techniques with Phonon Detection 59
3.1.2 Techniques with Photon Detection 60
3.1.2.1 X-Ray and ?-Ray Counting and Spectroscopy 60
3.1.2.2 From Scanning 1D to Mapping 2D 64
3.1.2.3 From Scanning 1D to Tomography 3D 65
3.1.2.4 From Static Source to Dynamic Source Counting 66
3.1.3 Techniques with Lepton Detection 68
3.1.3.1 Neutrino Counting and Spectroscopy 68
3.1.3.2 From Neutrino Counting to Tomography 70
3.1.3.3 Measurement of Redox Potential 71
3.1.3.4 Electron Counting and Spectroscopy 73
3.1.3.5 ??? 2D Autoradiography 76
3.1.3.6 Positron Emission Tomography 76
3.1.4 Techniques with Neutron Detection 78
3.1.5 Techniques with Atom or Ion Detection 79
3.1.5.1 Ion Sensitive Electrodes 79
3.1.5.2 ? Counting and Spectroscopy 80
3.2 Material Characterization by Field-Free Interactive Techniques 83
3.2.1 Techniques with Phonon Interaction and Phonon Detection 84
3.2.1.1 Phononic Acoustic Measure and Spectroscopy 85
3.2.1.2 Acoustic Microscopy 86
3.2.1.3 Seismic Reflection 88
3.2.2 Techniques with Photon Interaction and Phonon Detection 92
3.2.2.1 Laser Induced Photo-Acoustic Spectroscopy 92
3.2.2.2 Laser Induced Breakdown Spectroscopy (LIBS) 93
3.2.2.3 Performance of the Interactive Photon–Phonon Techniques 94
3.2.3 Techniques with Photon Interaction and Photon Detection 95
3.2.3.1 Ground Penetrating Radar 95
3.2.3.2 Infrared Spectroscopy 97
3.2.3.3 Diffuse Reflection Spectroscopy 99
3.2.3.4 Near Infrared—Visible—Ultraviolet Spectroscopy and Colorimetry 102
3.2.3.5 Single Particle Counting 107
3.2.3.6 Photon Correlation Spectroscopy 109
3.2.3.7 Raman Spectroscopy 110
3.2.3.8 Atomic Absorption Spectroscopy, Optical Emission Spectroscopy and Laser-Induced Breakdown Spectroscopy 113
3.2.3.9 Ultraviolet Fluorescence Spectroscopy 115
3.2.3.10 X-Ray Absorption and X-Ray Fluorescence Spectroscopy 119
3.2.3.11 X-Ray Fluorescence 121
3.2.3.12 X-Ray Absorption Fine Structure Spectroscopy 123
3.2.3.13 X-Ray Diffraction, Small Angle X-Ray Scattering and Laue Diffraction 131
3.2.3.14 X-Ray and ?-Ray Tomography 138
3.2.3.15 Analysis Using a Free-Electron Laser 140
3.2.3.16 Mössbauer Absorption 141
3.2.3.17 Photoactivation 145
3.2.3.18 Detection Limit for the Interactive Photon-Photon 146
3.2.4 Techniques with Photon Interaction and Lepton Detection 147
3.2.4.1 Ultraviolet and X-Ray Photoelectron Spectroscopy 147
3.2.4.2 Surface Extended X-Ray Absorption Fine Structure 148
3.2.5 Techniques with Photon Interaction and Ion or Neutron Detection 148
3.2.5.1 Photon-Induced Mass Spectroscopy 148
3.2.5.2 Laser Ablation Inductively Coupled Plasma Mass Spectrometry 149
3.2.5.3 Resonance Ionization Mass Spectroscopy 151
3.2.5.4 Laser microprobe mass analysis (LAMMA) 152
3.2.5.5 Photoactivation 153
3.2.6 Techniques with Lepton Interaction and Phonon Detection 154
3.2.6.1 Techniques with Electron Interaction and Phonons Detection 154
3.2.7 Techniques with Lepton Interaction and Photon Detection 155
3.2.7.1 Electron Probe Microanalysis 155
3.2.7.2 Positron Annihilation Lifetime Spectroscopy 158
3.2.8 Techniques with Lepton Interaction and Lepton Detection 162
3.2.8.1 Scanning Electron Microscopy 162
3.2.8.2 Transmission Electron Microscopy and Associated Techniques 163
3.2.8.3 Techniques with Muon Interaction and Muon Detection 169
3.2.9 Techniques with Lepton Interaction and Neutron Detection 173
3.2.10 Techniques with Lepton Interaction and Ion Detection 173
3.2.10.1 Electro-Spray Ionization Mass Spectroscopy 173
3.2.10.2 Spark Source Mass Spectroscopy 174
3.2.11 Techniques with Neutron Interaction and Photon Detection 174
3.2.11.1 Instrumental Neutron Activation Analysis 174
3.2.11.2 Radiochemical Neutron Activation Analysis 177
3.2.11.3 Activation Analysis with Fast Neutrons 177
3.2.12 Techniques with Neutron Interaction and Lepton Detection 178
3.2.13 Techniques with Neutron Interaction and Neutron Detection 181
3.2.13.1 Prompt Neutrons Spectroscopy 181
3.2.13.2 Delayed Neutrons Spectroscopy 182
3.2.13.3 Neutron Diffraction and Scattering 182
3.2.13.4 Neutron Radiography and Tomography 184
3.2.14 Techniques with Neutron Interaction and Ion Detection 186
3.2.14.1 Thermal Neutron-Induced Fission Track Technique 186
3.2.14.2 Fast Neutron-Induced Fission Track 187
3.2.14.3 Neutron Elastic Recoil Detection Analysis 189
3.2.15 Techniques with Ion or Atom Interaction and Phonon Detection 189
3.2.15.1 Interactive Atom-Phonon techniques 190
3.2.16 Techniques with Ion or Atom Interaction and Photon Detection 190
3.2.16.1 Inductively Coupled Plasma Atomic Emission Spectroscopy 191
3.2.16.2 Particle-Induced X-Ray Emission 192
3.2.16.3 Particle-Induced Gamma-Ray Emission 194
3.2.17 Techniques with Ion Interaction and Neutron Detection 194
3.2.18 Techniques with Ion or Atom Interaction and Ion Detection 195
3.2.18.1 Volumetric Analysis 195
3.2.18.2 Atom Force Microscopy 199
3.2.18.3 Micro- Nano-Indentation (NI) 202
3.2.18.4 Inductively Coupled Plasma Mass Spectrometry 204
3.2.18.5 Secondary Ion Mass Spectrometry 209
3.2.18.6 Accelerator Mass Spectrometry 212
3.2.18.7 Rutherford Back-Scattering Spectrometry 214
3.2.18.8 Elastic Recoil Detection Analysis 215
3.2.18.9 Nuclear Reaction Analysis 218
3.3 Material Characterization by Techniques Under Specific Field 220
3.3.1 Techniques with Field or Phonon Detection 220
3.3.1.1 Barkhausen Noise Analysis Under Magnetic Field 220
3.3.2 Techniques with Photon Detection 222
3.3.2.1 Mössbauer Emission Spectroscopy Under Magnetic Field 222
3.3.3 Techniques with Atom/Ion Detection 222
3.3.3.1 Gravimetry 222
3.3.4 Techniques with Photon Interaction and Photon Detection 224
3.3.4.1 Nuclear Magnetic Resonance 224
3.3.4.2 Solid-State Nuclear Magnetic Resonance 226
3.3.4.3 NMR 3D-Tomography 228
3.3.4.4 Electron Paramagnetic Resonance 229
3.3.4.5 X-Ray Magnetic Circular Dichroism 231
3.3.4.6 Photoelectron Emission Microscopy Spectroscopy 232
3.3.4.7 Mössbauer Absorption Spectroscopy 233
3.3.5 Techniques with Photon Interaction and Lepton Detection 234
3.3.6 Techniques with Lepton Interaction and Photon Detection 234
3.3.6.1 Muon Spin Spectroscopy 234
3.3.7 Techniques with Lepton Interaction and Lepton Detection 237
3.3.7.1 Energy-Loss Magnetic Chiral Dichroism 237
3.3.8 Techniques with Lepton Interaction and Ion Detection 238
3.3.8.1 Electrical Conductivity 239
3.3.8.2 Coulometry 241
3.3.8.3 Voltammetry 243
3.3.8.4 Polarography 247
3.3.8.5 Atom Probe Tomography 252
References 255
4 Comparing and Combining Analytical Techniques 278
4.1 Comparing Analytical Techniques 278
4.1.1 Comparing Passive Techniques 279
4.1.2 Comparing Interactive Techniques 280
4.1.2.1 Interaction-Detection: Options and Limitations 281
4.1.2.2 Elastic Interaction: Diffraction Techniques 281
4.1.2.3 Inelastic Interaction: Absorption/Fluorescence Techniques 282
4.1.3 Comparing Passive and Interactive Methods 283
4.1.3.1 Comparing Techniques for Characterization 283
4.1.3.2 Comparing Techniques for Imaging 286
4.1.3.3 Comparing Isotope and Element Analysis 287
4.1.4 Comparing the Detetion Limits and Relevant Issues 288
4.2 Combining Techniques 290
4.2.1 Combining Passive Techniques 290
4.2.2 Combining Interactive Techniques 291
4.2.2.1 Combining Photon-Photon Interactive Techniques 291
4.2.2.2 Combining Photon-Photon and Electron-Photon Interactive Techniques 293
4.2.2.3 Combining Other Interactive Techniques 294
4.2.3 Combining All Analytical Techniques 295
References 297
5 Concluding Summary 300
Index 305