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Tables of Contents for Non-Destructive Elemental Analysis
Chapter/Section Title
Page #
Page Count
Contributors
v
Introduction
1
3
Z.B. Alfassi
Nuclear activation analysis
4
54
Z.B. Alfassi
Introduction
4
1
Basic nuclear physics
5
14
Nuclides
6
1
Radioactive decay
6
4
Kinetics of decay of radioactive nuclides
10
1
Kinetics of chain decays
11
1
Kinetics of formation of radioactive nuclides by irradiation
11
6
The chart of the nuclides
17
2
Gamma detection systems
19
5
Nal(TI) scintillation detector
19
1
Solid-state ionization detector
20
4
The shape of the γ spectrum
24
4
Neutron sources
28
2
Samples introduction
30
1
Instrumental neutron activation analysis (INAA)
30
24
Techniques
30
1
Calculation
31
2
Calibration and calculation
33
2
Nuclear interferences
35
1
A special case - INAA of trace elements in silicon
36
3
A suggested procedure for a general case
39
4
An example of interferences removal in INAA - determination of Pt in aerosols
43
3
Epithermal INNA
46
3
Thermal neutron absorbers
49
2
Fast-neutron INAA
51
1
Determination of phosphorus and silicon
51
1
Neutron activation analysis with emissions other than γ emission
52
1
β-
52
1
X-rays
52
1
Neutrons
53
1
Depth profiling by INAA
53
1
Charged-particle activation analysis (CPAA)
54
4
References
55
3
Prompt gamma-neutron activation analysis with reactor neutrons
58
57
C. Yonezawa
Introduction
58
1
History of reactor-based PGNAA
58
1
Principles and characteristics
59
3
Principles
59
1
Neutron capture reaction and prompt γ-rays
60
2
Characteristics of PGNAA
62
1
Facilities
62
15
Types of reactor-based facilities
62
2
Internal target type facilities
64
1
External target type facilities
65
2
Low-energy guided neutron beam type facilities
67
4
Creation of a neutron beam
71
1
Conventional thermal neutron beam
71
1
Guided neutron beam
71
1
Cold neutron source
72
1
Radiation shielding and sample support
73
2
The γ-ray spectrometer
75
2
Elemental analysis
77
24
Basics for elemental analysis
77
1
Analytical sensitivity and detection limit
77
5
Doppler broadening of the B 478 keV γ-ray
82
2
Spectral interference
84
1
Effects of neutron absorption and scattering
85
5
γ-ray attenuation
90
1
γ-ray background
90
2
Prompt γ-ray data
92
2
γ-ray spectrum analysis
94
2
Standardization
96
1
Introduction of standardization
96
1
Comparative method
97
1
Standardization based on an internal standard method
98
3
Applications
101
6
Hydrogen analysis
101
1
Boron analysis
102
2
Other elements
104
3
Isotopic analysis
107
1
New techniques for PGNAA
107
8
References
111
4
Elemental analysis by laser ablation ICP-MS
115
36
T.E. Jeffries
Introduction
115
1
Background
116
2
Laser ablation
116
1
ICP-MS
117
1
Instrumentation
118
14
ICP-MS
119
1
The inductively coupled plasma (ICP)
120
1
The plasma sampling interface
121
1
Ion focusing
122
1
The quadrupole mass analyser
122
1
Ion detection and signal handling
123
1
Laser
124
1
The Nd: YAG laser and flashlamp
124
2
The laser cavity and lasing event
126
1
Harmonic generation (frequency quadrupling)
127
1
Harmonic separation
128
1
Energy control and focusing
128
1
Sample viewing and movement
129
1
Ablation cell
130
1
Sample transport
131
1
Analytical technique
132
10
Sample preparation
132
2
Factors affecting analysis
134
1
ICP-MS parameters
134
1
Laser parameters
135
1
Laser-induced elemental fractionation
136
1
Instrumental optimisation and calibration
137
1
Optimisation (tuning)
137
1
Calibration
137
2
Data collection and handling
139
1
Data collection
139
2
Data handling
141
1
Applications
142
2
Literature reviews
142
1
Geological, earth and planetary sciences applications
142
1
Life and environmental sciences applications
143
1
Archaeological and palaeontological sciences applications
144
1
Forensic science applications
144
1
Materials science applications
144
1
Continuing developments and final comments
144
1
Continuing developments
144
1
Final comments
145
1
Questions and answers
145
6
Questions and problems
145
1
Suggested answers
145
2
References
147
4
X-ray fluorescence
151
28
J. Injuk
R. Van Grieken
Introduction
151
1
History of X-rays
151
1
Properties of X-rays
152
5
Characteristic radiation
152
2
Continuum
154
1
Attenuation of X-rays
155
2
X-ray sources
157
1
Dispersing systems and detection of X-rays
158
2
Sample preparation methods
160
5
X-ray fluorescence techniques
165
12
Wavelength-dispersive X-ray fluorescence (WDXRF)
165
1
Applications, calibration and matrix effects
166
2
Energy-dispersive X-ray fluorescence (EDXRF)
168
1
Applications, calibration and matrix effects
169
2
Total-reflection X-ray fluorescence (TXRF)
171
2
Applications and calibration
173
2
Micro-X-ray fluorescence analysis (Micro-XRF)
175
1
Applications
176
1
Conclusions, trends and the future
177
2
References
178
1
Elemental analysis in scanning electron microscopy
179
22
M. Talianker
Generation of X-ray radiation in scanning electron microscope
179
2
Spectral notation of X-ray emission lines
181
1
The penetration of beam electrons into a bulk specimen: spatial resolution of X-ray microanalysis
182
2
Collection of X-rays in SEM: energy resolution
184
7
The wavelength-dispersive spectrometer
184
4
The energy-dispersive spectrometer
188
3
Quantitative micro-analysis in SEM
191
8
ZAF correction method
192
1
The atomic number effect
192
4
The absorption effect
196
1
The fluorescence effect
197
1
The peak-to-local continuum method
198
1
Summary
199
2
References
199
2
Elemental analysis by AES, XPS and SIMS
201
32
H.J. Mathieu
Introduction
201
1
Electron spectroscopies
202
21
X-ray photoelectron spectroscopy (XPS)
203
11
Auger electron spectroscopy (AES)
214
3
Sputter depth profiling with AES and XPS
217
6
Secondary ion mass spectrometry (SIMS)
223
7
Summary
230
1
Acknowledgements
231
2
References
231
2
Charged particle-induced X-ray emission
233
43
R.D. Vis
Introductory remarks
233
1
History
233
1
Introduction
234
1
Theory
234
4
The cross-section for inner-shell ionisation by ions
234
1
The binary encounter approximation (BEA)
234
1
The plane wave Born approximation (PWBA)
235
1
The semi-classical approach (SCA)
235
1
The ECPSSR theory
236
1
The fluorescence yield
236
2
The sensitivity and detection limits of PIXE
238
4
The optimal bombarding energy
238
1
The definition of the sensitivity
239
1
The production of background
240
1
The detection limit
241
1
The accuracy and precision of PIXE
242
2
The sources of error
242
1
Random errors
242
1
Systematic errors
243
1
The experimental set-up
244
6
The accelerator
244
1
The sample chamber
244
2
The detector(s)
246
1
Special geometries
246
1
External beams
246
1
Glancing incident beams
247
1
Glancing exit geometry
247
2
The data-handling system and software
249
1
Data acquisition
249
1
The software
249
1
Sample preparation and sample damage
250
6
General considerations
250
1
Standard PIXE
251
1
Micro-PIXE
252
2
Samples for GIPIXE and GEPIXE
254
1
Sample damage during irradiation
254
1
Definition
254
1
Heat effects
255
1
Effects of radiation dose
255
1
Other effects of the beam
255
1
Applications
256
12
General remarks
256
1
Biomedical applications
257
1
Macro-PIXE
257
3
Micro-PIXE
260
2
Environmental applications
262
1
Macro-PIXE
262
1
Micro-PIXE
263
1
Applications in geology
264
1
Macro-PIXE
264
1
Micro-PIXE
265
1
Miscellaneous applications
266
1
Applications in arts and archaeology
266
1
Applications in materials science
267
1
Conclusions and future prospects
268
8
PIXE amidst other methods for elemental analysis
268
2
Future prospects
270
2
References
272
4
Charged particle-induced γ-ray emission
276
32
J. Raisanen
Introduction
276
1
Nuclear reactions
277
1
Resonance capture
277
1
Inelastic scattering
277
1
Rearrangement collision
277
1
Thick target γ-ray yields
278
3
γ-ray yield from a thick target
278
1
Stopping power correction
279
2
Experimental considerations
281
6
Points to be taken into account
281
1
Geometry
281
1
Background spectra
282
1
Peak broadening
283
1
Energy and absolute efficiency calibration
284
1
Experimental arrangements
285
1
In vacuum arrangements
285
1
External beams
286
1
PIGE with micro-beams and other specialised equipment
286
1
Particle-induced thick target γ-ray yields and bombarding particle choice
287
14
Proton-induced γ-ray yields
287
8
Low-yield elements
295
1
Deuteron- and triton-induced γ-ray yields
295
1
Deuterons
295
2
Tritons
297
1
&alpah; Particle-induced γ-ray yields
297
2
Low-yield elements
299
1
Lithium-induced y-ray yields
299
1
Low-yield elements
300
1
Heavy ion-induced γ-ray yields
300
1
12C, 14N and 16O ion-induced γ-ray yields
300
1
55Cl ion-induced γ-ray yields
300
1
Selected applications of PIGE
301
3
Fluorine determination
302
1
Channelling measurements with PIGE
302
1
Analysis of the major structural elements in biomedical samples
302
1
Miscellaneous applications
303
1
Advantages and limitations of PIGE
304
4
References
304
2
Exercises and questions
306
2
Nuclear reaction analysis
308
31
D.J. Cherniak
W.A. Lanford
Introduction
308
1
Q values and cross-sections
309
3
Resonant nuclear reaction analysis
312
10
15N resonant nuclear reaction analysis measurement of hydrogen profiles
312
4
Depth scale
316
1
Concentration scale
316
1
Depth resolution
317
1
Sensitivity
317
1
Other light elements profiled by resonant nuclear reaction analysis
317
1
Applications - resonant profiling
318
1
Kinetics of H-ion implantation-induced blistering of semiconductors (H profiles)
318
1
H in amorphous Si solar cell materials
318
1
Study of the reaction between water and glass (Na and H profiles)
318
1
Fluorine in low-k dielectrics (F profiles)
319
2
Study of N-ion implantation into metal (15N profiles)
321
1
Migration of Li in electrochromic windows (Li profiles)
321
1
Non-resonant profiling
322
9
Fundamental aspects of non-resonant profiling
323
1
Depth scale
323
2
Concentration scales
325
1
Depth resolution
325
1
Sensitivity
326
1
Standards
327
1
Applications - non-resonant NRA
327
1
Oxygen diffusion in rutile
328
1
Oxygen diffusion in sapphire
328
1
Residual carbon in ceramic substrates
328
1
Sulfur in bulk CdTe and CdTe/CdS thin-film heterojunctions
328
1
Silicon diffusion in gold
329
2
Uranium dioxide corrosion
331
1
Multiple probes for light element analysis
331
4
Summary
335
4
References
335
4
Backscattering and forward scattering for depth profiling of solids
339
47
G. Demortier
G. Terwagne
Introduction
339
1
Position of RBS and ERD in comparison with other IBA techniques
340
7
Kinematics of RBS
347
3
The scattering cross-sections
350
2
Rutherford cross-sections
350
1
Non-Rutherford cross-sections
351
1
Typical RBS spectra for thin layers
352
5
Experimental arrangement
357
3
Calculation of RBS spectra
360
2
Contribution of non-Rutherford scattering
362
1
Fundamentals of ERD
363
3
Selected applications
366
20
Characterisation of the interdiffusion in Au-Al layers
366
4
RBS study of layers on spherical samples
370
1
Bulk analysis of ancient gold artefacts
371
2
Depth profiling light elements near an interface
373
2
Sodium profiling
375
1
Fluorine profiling
375
3
Light elements analysis of nitrogen-implanted aluminium
378
1
Depth profiling measurements
378
1
Rutherford backscattering measurements
378
2
High-resolution depth profiling of light and heavy elements in multilayers by using 3He particles
380
1
Combining RBS and NRA techniques
381
2
ERD technique
383
1
Steel surfaces modified by ion implantation
383
2
References
385
1
Experimental data analysis
386
50
M. Aboudy
Z.B. Alfassi
Introduction
386
1
Properties of a population
386
3
Random variable and distribution
386
1
Probability function and probability density function
386
2
Properties of distributions
388
1
Important distribution
389
13
Discrete distributions
389
1
Binomial distribution
389
1
Hypergeometric distribution
390
2
Poisson distribution
392
1
Continuous distribution
392
1
Normal distribution
392
4
Chi-square distribution
396
3
t (Student's) distribution
399
1
F Distribution
400
2
Properties of a sample
402
4
Sample mean
404
1
Sample variance
405
1
Confidence interval
406
12
Confidence interval for the mean with known population variance (σ2)
407
1
Confidence interval for the mean with unknown population variance
408
4
Confidence interval for the difference of means with known population variances
412
1
Confidence interval for the difference of means with unknown population variances
413
3
Confidence interval for population variance
416
1
Confidence interval for ratio of variances
416
2
Hypothesis and significance tests
418
4
Test of hypothesis for population mean (μ)
419
1
Test of hypothesis for difference of means
420
1
Test of hypothesis for population variance
421
1
Test of hypothesis for comparing two population variances
422
1
Outliers
422
4
Introduction
422
1
Dixon's Q test
423
1
Grubb's test for outliers
423
1
Youden's test for outlying laboratories
424
2
Calibration curves
426
10
Standards for calibration curves
426
1
Derivation of an equation for the calibration curves
426
2
Test for linearity
428
2
Calculation of a concentration
430
1
Weighted least squares linear regression
431
1
Non-linear calibration equations
431
1
Calibration curves in activity measurements
432
1
Calibration curves for neutron capture radiography
433
2
Limit of detection
435
1
References
435
1
Index
436