Atomic Spectroscopy in Elemental Analysis

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ISBN: 9781841273334 | 1841273333
Cover: Hardcover
Copyright: 8/1/2003

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tomic spectroscopy is the key technology used in the characterisation of inorganic materials. It encompasses a wide variety of techniques and provides rapid, sensitive and selective determination of elemental composition.his volume provides an overview of the complete range of atomic spectroscopy techniques available to the elemental analyst. Each chapter covers the essential principles of a technique, the available instrumentation and a range of representative applications.his is a book for analytical chemists, environmental chemists, earth scientists, food scientists and petrochemists in the industrial and academic sectors.

Contributors	p. xi
Preface	p. xiii
Method validation for atomic spectroscopy	p. 1
Introduction	p. 1
The process	p. 2
Create the validation plan	p. 3
Precision	p. 4
Bias	p. 10
Ruggedness	p. 12
Limit of detection, limit of quantification and selectivity	p. 13
The working range and linearity	p. 15
Equipment qualification	p. 17
Assessment of uncertainty	p. 19
Has the method met the requirements set out in the validation plan?	p. 21
Acknowledgements	p. 21
References	p. 22
Inductively coupled plasma mass spectrometry	p. 23
Introduction	p. 23
History and development	p. 24
Instrumentation	p. 24
Sample introduction	p. 24
Plasma	p. 26
Interface	p. 28
Vacuum system	p. 30
Ion focusing	p. 30
Collision cells	p. 32
Mass analyser	p. 35
Detector	p. 38
Operation	p. 39
Sample preparation and introduction	p. 39
Plasma optimisation	p. 40
Control of interferences	p. 41
Data acquisition	p. 44
Calibration and quantification	p. 45
Applications	p. 46
Environment, agriculture and food	p. 46
Semiconductor	p. 48
Clinical and pharmaceutical	p. 49
Geological and nuclear	p. 49
Forensic and archaeological	p. 50
Chemical, petrochemical and material testing	p. 50
Acknowledgements	p. 51
References	p. 51
Inductively coupled plasma atomic emission spectrometry	p. 55
Introduction	p. 55
Theory	p. 55
How a plasma is formed?	p. 55
Atomic emission theory	p. 56
Interferences	p. 59
Instrumentation	p. 61
Generators	p. 61
Line isolation devices	p. 62
Detectors	p. 65
Radial and axial ICPs	p. 68
Sample introduction	p. 69
Nebulisers and spray chambers	p. 69
Torches	p. 73
Other sample introduction methods	p. 77
Applications	p. 80
Simple applications	p. 81
Pre-concentration methods	p. 82
Speciation and coupled techniques	p. 83
Analysis of gases and high resolution applications	p. 85
Alternative plasmas	p. 85
Chemometrics and data manipulation	p. 86
Conclusions	p. 87
References	p. 88
Analytical glow discharges	p. 91
Introduction	p. 91
Basic principles of the analytical GD	p. 91
Introduction	p. 91
Typical discharge conditions of analytical GD	p. 93
Spatial regions in the analytical GD	p. 95
Species present in the analytical GD	p. 98
Most important collision processes in the plasma	p. 104
Elastic collisions	p. 106
Ionization and excitation of argon atoms	p. 106
Ionization and excitation of sputtered (analyte) atoms	p. 109
Positive ion-electron recombination	p. 111
De-excitation	p. 113
Processes occurring at the walls	p. 114
Secondary electron emission	p. 114
Sputtering	p. 116
Glow discharge optical emission spectroscopy	p. 120
Introduction	p. 120
Source and instrumental development	p. 121
Quantitative depth profile analysis	p. 122
Application of a CCD detector	p. 125
Radio frequency GD and interference effect	p. 127
Quantification approaches and measurement of electrical parameters	p. 131
Glow discharge mass spectrometry	p. 132
Source and instrumental development	p. 133
Instrumentation	p. 137
Sample preparation	p. 140
Quantification	p. 141
Analytical figures of merit	p. 143
Sensitivity	p. 143
Limit of detection	p. 143
Reproducibility and precision	p. 144
Robustness	p. 144
Accuracy	p. 144
Applications	p. 145
Bulk analysis of conducting and semi-conducting samples	p. 147
Bulk analysis of non-conducting samples	p. 148
In-depth analysis of surface layers	p. 148
Conclusion	p. 152
References	p. 152
Microwave plasma atomic emission spectroscopy	p. 157
Introduction	p. 157
Microwave-induced plasmas (MIP)	p. 157
MIPs as chromatographic detectors	p. 159
Analytical information from GC-AED	p. 166
GC-AED detection of non-metallic elements	p. 168
GC-AED detection of metallic elements	p. 172
Main group metallic compounds	p. 172
GC-AED of transition metal compounds	p. 175
Isotope detection by GC-AED	p. 181
Analytical derivatization in GC-AED	p. 182
Liquid and supercritical fluid chromatographic applications of AED detection	p. 183
The role and future development of MIP-AED chromatographic detection	p. 185
References	p. 185
X-ray fluorescence analysis (XRF)	p. 189
Introduction	p. 189
Physics of X-ray absorption and excitation	p. 189
Introduction	p. 189
Absorption	p. 190
The photoelectric effect	p. 191
Scattering of X-rays	p. 193
Nomenclature of characteristic X-rays	p. 194
The fluorescence yield	p. 194
Excitation of X-rays	p. 195
Radio-isotopes	p. 195
X-ray tubes	p. 196
Synchrotron radiation	p. 197
Principal components of wavelength dispersive XRF spectrometers	p. 198
Introduction	p. 198
Bragg's law for diffraction	p. 199
Analyzer crystal	p. 201
Goniometer	p. 203
Collimators	p. 204
Detectors	p. 204
Gas-filled detectors	p. 205
Scintillation detectors	p. 207
Other arrangements	p. 207
Principal components of EDS	p. 208
Introduction	p. 208
Detectors	p. 209
Introduction	p. 209
Si(Li) detectors	p. 209
Si-PIN detectors	p. 209
Si-drift chamber detectors	p. 210
High-resolution detectors	p. 210
Applications	p. 210
Qualitative analysis	p. 210
Quantitative analysis	p. 211
Absorption	p. 211
Enhancement	p. 213
Correction for matrix effects	p. 215
Fundamental parameter method	p. 215
Compton correction	p. 215
Influence coefficient algorithms	p. 216
Notes on specimen preparation	p. 217
Conclusion	p. 218
References	p. 218
Electrothermal atomic absorption spectrometry	p. 221
Introduction	p. 221
Graphite atomizers	p. 222
Graphite furnace analysis	p. 225
Drying	p. 226
Pyrolysis	p. 227
Cool-down (optional)	p. 227
Atomization	p. 227
The clean out	p. 228
Electrothermal atomization	p. 228
Interferences in graphite furnace AAS	p. 232
The relative merits of ETAAS	p. 237
References	p. 238
Flame atomic absorption spectroscopy, including hydride generation and cold vapor techniques	p. 239
Introduction	p. 239
Why flame atomic absorption spectrometry?	p. 239
The current status of FAAS	p. 240
Closely related techniques: hydride generation, cold vapor mercury, AFS and AES	p. 241
Basic principles	p. 242
How do FAAS instruments work?	p. 244
Sample introduction	p. 245
Nebulizers	p. 245
Spray chamber	p. 246
Flames	p. 246
Light sources	p. 248
Atom source emission	p. 250
Stray radiation	p. 250
Detectors	p. 251
Optical system	p. 252
Instruments for hydride generation	p. 253
Instruments for cold vapor mercury determination	p. 254
Instruments for AFS	p. 255
Limitations to performance	p. 256
Instrument effects	p. 257
Analyte effects (or why all elements do not have the same detection limit)	p. 258
Sample effects	p. 259
How to get the right answer?	p. 260
How to deal with interference effects?	p. 260
Separation and preconcentration	p. 262
Flow injection techniques	p. 264
Other possibilities for improving analytical performance	p. 264
Some practical points	p. 265
Safety	p. 265
Nebulizers (sensitivity drift)	p. 266
Light sources	p. 266
Calibration	p. 266
Achieving very low detection limits	p. 267
Sample preparation issues	p. 267
Representative applications	p. 268
Earth sciences	p. 268
Environmental	p. 270
Petroleum related	p. 273
Food and beverages	p. 274
Clinical and forensic	p. 276
Bibliography	p. 277
References	p. 279
Chemometrics in elemental analysis	p. 282
Introduction	p. 282
Experimental design and optimization	p. 282
Multi-variate statistics	p. 288
Exploratory data analysis	p. 293
Cluster analysis	p. 293
Principal components analysis	p. 295
Discriminant analysis	p. 299
Calibration models	p. 301
Conclusion	p. 306
References	p. 306
Index	p. 308
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