Chemical Analysis: Modern Instrumental Methods and Techniques, English Edition

by Francis Rouessac; Annick Rouessac

ISBN13: 9780471972617

ISBN10: 0471972614

Format: Paperback

Pub. Date: 2000-06-01

Publisher(s): WILEY

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Summary

Chemical Analysis is an essential introduction to a wide range of analytical techniques and instruments. Assuming little in the way of prior knowledge, this text carefully guides the reader through the more widely used and important techniques, whilst avoiding excessive technical detail. Covering both instrumental techniques and the situations in which they are used, the text always strives to maintain a balance between breadth and depth of coverage. Carefully structured, this book clearly differentiates between separation and spectral methods, and includes a section on more specialised techniques. Chemical Analysis * Provides a through introduction to a wide range of the most important and widely used instrumental techniques. * Maintains a careful balance between depth and breadth of coverage. * Includes many examples, problems and their solutions. Chemical Analysis will be invaluable to those studying or using instrumental techniques throughout the sciences, medicine and engineering.

Foreword to the French edition

xiii

Foreword to the English edition

xiv

Preface to the French edition

Preface to the English edition

xvii

Acknowledgements

xix

Introduction

xxi

PART 1 SEPARATION METHODS

(124)

General aspects of chromatography

(20)

General concepts of analytical chromatography

(1)

Classification of chromatographic techniques

(2)

The chromatogram

(2)

The ideal chromatogram and Gaussian peaks

(1)

Real peaks

(1)

The theoretical plate model

(3)

Column efficiency

(1)

Retention parameters

(2)

Separation factor between two solutes

(1)

Resolution factor between two peaks

(1)

The van Deemter equation in gas chromatography

(2)

Optimisation of a chromatographic analysis

(4)

Problems

(2)

Gas chromatography

(22)

Components of a gas chromatograph

(2)

Carrier gas and flow regulation

(1)

Sample introduction and injection chamber

(2)

Oven

(1)

Columns

(3)

Stationary phases (liquid type)

(2)

Stationary phases (solid type)

(1)

Common detectors

(4)

Detectors yielding structural information

(2)

Appendix - Retention indices and constants related to stationary phases

(1)

Kovats relationship

(1)

Kovats retention indices

(1)

Stationary phase constants

(5)

Problems

(3)

High performance liquid chromatography

(20)

Origin of HPLC

(1)

General scheme of an HPLC system

(1)

Pumps and gradient elution

(2)

Injectors

(1)

Columns

(1)

Stationary phases

(3)

Mobile phases

(2)

Chiral chromatography

(1)

Principal detectors

(6)

Applications

(3)

Problems

(3)

Ion chromatography

(20)

The principle of ion chromatography

(1)

Mobile phases

(1)

Stationary phases

(2)

The principle of separation

(2)

Conductivity detectors

(1)

Ion suppressors

(3)

Appendix - Quantitative analysis by chromatography

(1)

Principle and basic equation

(1)

Recording integrators and data treatment software

(2)

External standard method

(1)

Internal standard method

(2)

Internal normalisation

(5)

Problems

(4)

Planar chromatography

(10)

Planar chromatography: principles of application

(1)

Post-chromatography: development of the plate

(1)

Stationary phases

(1)

Retention and separation parameters

(1)

Quantitative TLC

(1)

Aspects of TLC

(5)

Problems

(2)

Supercritical fluid chromatography

(6)

Supercritical fluids

(1)

Supercritical phases as mobile phases

(1)

Comparison of SFC with HPLC and GC

(1)

Instrumentation

(1)

SFC in chromatographic techniques

(2)

Size exclusion chromatography

101

(10)

The principle of SEC

101

(1)

Stationary phases

102

(2)

Instrumentation

104

(1)

Domains of application

105

(6)

Problems

109

(2)

Capillary electrophoresis

111

(14)

Zone electrophoresis

111

(2)

Free solution capillary electrophoresis

113

(1)

Electrophoretic mobility and electro-osmotic How

114

(3)

Instrumentation and techniques

117

(2)

Indirect detection

119

(1)

Performance of capillary electrophoresis

119

(6)

Problems

121

(4)

PART 2 SPECTROSCOPIC METHODS

125

(162)

Nuclear magnetic resonance spectroscopy

127

(34)

General description

127

(1)

Spin/magnetic field interaction for a nucleus

128

(2)

Nuclei that can be studied by NMR

130

(1)

Bloch's theory for a nucleus of I = 1/2

130

(2)

Larmor's frequency

132

(2)

Chemical shift

134

(1)

The principle of obtaining an NMR spectrum

135

(2)

Relaxation processes

137

(1)

The measurement of chemical shifts

138

(1)

Shielding and deshielding of the nuclei

139

(1)

Factors influencing chemical shifts

140

(2)

Hyperfine structure: spin/spin coupling

142

(1)

Heteronuclear coupling

142

(3)

Homonuclear coupling

145

(3)

Spin decoupling and modes of operation

148

(2)

Fluorine and phosphorous NMR

150

(1)

Appendix - Quantitative NMR

151

(1)

Measurement of area - application to simple analysis

151

(1)

Samples containing compounds that can be identified

152

(1)

Internal standard method

153

(1)

Standard additions method

154

(1)

Analysers using pulsed NMR

155

(6)

Problems

158

(3)

Infrared spectroscopy

161

(28)

Spectral representation in the mid infrared (IR)

161

(1)

Origin of absorption bands in the mid infrared

162

(1)

Rotational-vibrational bands in the mid infrared

163

(1)

Simplified model for vibrational interactions

163

(2)

Real model (or vibrational interactions

165

(1)

Rotational bands of compounds in the gas phase

166

(1)

Characteristic bands for organic compounds

167

(1)

Instrumentation

168

(6)

Optics, sources and detectors used in the mid infrared

174

(2)

Sample analysis techniques

176

(4)

Infrared microscopy

180

(1)

Archiving spectra

181

(1)

Comparison of spectra

182

(1)

Calibration of cell thickness

183

(1)

Raman diffusion

184

(5)

Problems

186

(3)

Ultraviolet and Visible absorption spectroscopy

189

(32)

General concepts

189

(2)

Molecular absorptions

191

(1)

Origin of absorption in relation to molecular orbitals

192

(2)

Donor-acceptor association

194

(1)

Isolated chromophores

194

(1)

Solvent effects: solvatochromism

195

(1)

Chromophores in conjugated systems

196

(1)

Woodward-Fieser rules

197

(1)

UV/Visible spectrophotometers

198

(6)

Quantitative analysis in the UV/Visible

204

(1)

Beer-Lambert's law

205

(2)

Visual colorimetry

207

(1)

Absorbance measurements

208

(2)

Confirmation analysis (purity control)

210

(1)

Distribution of relative errors due to instruments

211

(1)

Baseline correction

212

(1)

Multicomponent analysis (MCA)

213

(2)

Derivative spectrometry

215

(6)

Problems

218

(3)

Fluorimetry

221

(16)

Fluorescence and phosphorescence

221

(1)

Origin of fluorescence

222

(2)

Fluorescence intensity

224

(2)

Rayleigh and Raman bands

226

(1)

Instrumentation

227

(3)

Applications

230

(1)

Chemiluminescence

231

(6)

Problems

233

(4)

X-ray fluorescence spectrometry

237

(16)

General principle

237

(1)

X-ray fluorescence spectrum

238

(1)

Excitation modes of elements in X-ray fluorescence

239

(3)

X-ray absorption

242

(1)

Sample preparation

242

(1)

Different types of instruments

243

(4)

Quantitative analysis by X-ray fluorescence

247

(1)

X-ray fluorescence applications

248

(5)

Problems

249

(4)

Atomic absorption and flame emission spectroscopy

253

(20)

Principles common to the two methods

253

(1)

Interpretation of the phenomena involved

254

(1)

Atomic absorption vs flame emission

255

(2)

Measurements by absorption or flame emission

257

(1)

Basic instrumentation for atomic absorption

258

(4)

Flame photometers

262

(2)

Correction of interfering absorptions

264

(4)

Physical and chemical interferences

268

(1)

Sensitivity and detection limits in AAS

269

(4)

Problems

271

(2)

Atomic emission spectroscopy

273

(14)

Optical emission spectrophotometry (OES)

273

(1)

Excitation by inductively coupled plasma (ICP)

274

(1)

Ionisation by are, spark or electronic impact

275

(2)

The principles o( atomic emission analysis

277

(1)

Spectral lines

277

(1)

Simultaneous and sequential instruments

278

(3)

Performance

281

(2)

GC coupled to atomic emission relatively

283

(1)

Applications of atomic emission spectrometry

283

(4)

Problems

284

(3)

PART 3 OTHER METHODS

287

(114)

Mass spectrometry

289

(40)

Principles

289

(3)

The Bainbridge spectrometer

292

(1)

Magnetic analysers (EB type)

293

(4)

Time of flight (TOF) analysers

297

(2)

Ion cyclotron resonance

299

(2)

Quadrupole analysers

301

(3)

Ion traps

304

(1)

Performance of mass spectrometers

305

(1)

Sample introduction

306

(1)

Major ionisation techniques (under vacuum)

307

(4)

Atmospheric pressure ionisation (API)

311

(3)

Ion detection

314

(1)

Tandem mass spectrometry

315

(2)

Appendix - Applications in mass spectrometry

317

(1)

Determination of empirical formulae

317

(1)

Determination of isotope ratios for an element

318

(2)

Identification using spectral libraries

320

(1)

Fragmentation of organic ions

321

(8)

Problems

325

(4)

Labelling methods

329

(18)

Principle of labelling methods

329

(1)

Isotopic dilution with a radioactive label

330

(1)

Measurement of radioisotope activity

331

(3)

Choice of a sub-stoichiometric method

334

(1)

Labelling with stable isotopes

334

(1)

Immunoenzymatic (IEA) methods of measurement

335

(4)

Other immunoenzymatic techniques

339

(1)

Advantages and limitations of the ELISA test in chemistry

340

(1)

Radio-immunoassay (RIA)

340

(1)

Immunofluorescence assay (IFA)

341

(1)

Neutron activation analysis (NAA)

341

(1)

Thermal neutrons

342

(1)

Induced activity - irradiation time

342

(1)

Detection by γ-counting - measurement principle

343

(1)

Applications

343

(4)

Problems

344

(3)

Potentiometric methods

347

(12)

General principles

347

(2)

A particular ion selective electrode: the pH electrode

349

(1)

Ion selective electrodes

350

(3)

Calculations and different methods

353

(3)

Applications

356

(3)

Problems

356

(3)

Coulometric and voltammetric methods

359

(18)

General principles

359

(1)

Dropping-mercury electrode

360

(1)

Continuous rent polarography

361

(1)

Diffusion current

362

(1)

Pulse polarography

363

(1)

Amperometric detection in HPLC and CE

364

(1)

Special sensors

365

(2)

Stripping voltammetry

367

(1)

Coulometric measurements

368

(1)

Karl Fischer coulometric determination of water

369

(3)

Determination by the Karl Fischer method

372

(5)

Problems

374

(3)

Some sample preparation methods

377

(8)

Evolution of methods

377

(1)

Solid-phase extraction using column or discs

378

(1)

Gas-solid extraction using columns or discs

379

(2)

Headspace sample analysis

381

(2)

Supercritical fluid extraction (SFE)

383

(1)

Mineralisation by microwave digestion

384

(1)

Basic statistical parameters

385

(16)

Mean value and accuracy

385

(1)

Precision and standard deviation of a group of results

386

(2)

Indeterminate or random errors

388

(2)

Confidence interval

390

(1)

Parametric tests - comparison of results

391

(2)

Rejection criteria - Q test (Dixon test)

393

(1)

Linear regression

394

(2)

Robust methods

396

(1)

Method optimisation using factorial analysis

397

(4)

Problems

398

(3)

Solutions

401

(34)

Appendix - List of acronyms

435

(2)

Bibliography

437

(2)

Table of physico-chemical constants

439

(2)

Index

441

Chemical Analysis: Modern Instrumental Methods and Techniques, English Edition

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