Spectrochemical analysis by atomic absorption and emission / L.H.J. Lajunen and P. Per̈am̈aki.

Format:

Book

Author/Creator:

Lajunen, Lauri H. J.

Contributor:

Perämäki, P.

Royal Society of Chemistry (Great Britain)

Alumni and Friends Memorial Book Fund.

Language:

English

Subjects (All):

Atomic absorption spectroscopy.

Atomic emission spectroscopy.

Physical Description:

xiii, 342 pages : illustrations ; 24 cm

Edition:

Second edition.

Place of Publication:

Cambridge : Royal Society of Chemistry, [2004]

Summary:

Atomic spectrometric techniques and ICP-MS are frequently used in trace element analysis in many laboratories. For those using them, or utilizing the analysis results obtained, it is essential to understand about the instrumental methods involved.

Spectrochemical Analysis by Atomic Absorpition and Emission provides this knowledge, by describing both the theory of atomic spectroscopy and all the major atomic spectrometric techniques (AAS, Flame-AES, Plasma AES, AFS, and ICP-MS), including basic concepts, instrumentation and applications.

Revised and fully updated, the book continues to be highly practical and wide in scope and to contain illustrations which aid understanding. Spectrochemical Analysis by Atomic Absorption and Emission is ideal for students and their lecturers, but will also be useful for practitioners who already use the techniques but would like to know more about the insides of the 'black box'.

Contents:

1.1 Historical 1

1.2 The Present Status of Atomic Spectrometric Methods 3

1.3.2 Terms Concerned with the Analytical Technique and Spectral Radiation 14

Chapter 2 Overview of Atomic Spectrometric Techniques 16

2.1 Theory of Atomic Spectroscopy 16

2.1.1 Atomic Absorption, Emission, and Fluorescence Spectra 16

2.1.2 Emission and Absorption of Energy 21

2.1.3 The Maxwell-Boltzmann Law 25

2.1.4 Spectral Linewidths 27

2.1.4.1 Natural Line Broadening 28

2.1.4.2 Doppler Broadening 29

2.1.4.3 Pressure Broadening 30

2.1.5 The Zeeman Effect 31

2.1.6 The Absorption Coefficient 34

2.1.7 Basic Concepts of the Plasma 36

2.2 Instrument Components 37

2.2.1 Radiation Sources 39

2.2.1.1 Hollow Cathode Lamps 39

2.2.1.2 Electrodeless Discharge Lamps (EDLs) 43

2.2.1.3 Microwave EDLs 43

2.2.1.4 Radiofrequency EDLs 44

2.2.2 Monochromator 44

2.2.2.1 Prism and Grating 46

2.2.3 Detectors 47

2.3 Sample Introduction in Atomic Spectrometry 52

2.3.1 Solution Nebulization 53

2.3.2 Introduction of Gaseous Samples 55

2.3.2.1 Hydride Generation 55

2.3.2.2 Cold Vapour Technique 63

2.3.2.3 Generation of Other Gaseous Species 65

2.3.3 Flow Injection Analysis 65

2.3.3.1 FIA-FAAS 66

2.3.3.2 FIA-Hydride Generation and FIA-Cold Vapour Techniques 66

2.3.3.3 Amalgamation 67

2.4 Calibration 68

2.4.1 Calibration Graph Method 68

2.4.2 Bracketing Method 72

2.4.3 Standard Addition Method 73

2.4.4 Internal Standards 73

2.4.5 Calibration Standards 74

2.4.5.1 Standard Solutions 74

2.4.5.2 Non-Aqueous Standards 75

2.4.6 Precision and Accuracy 76

Chapter 3 Atomic Absorption Spectrometry 78

3.1 Instrumentation 78

3.1.1 Basic Features of the Atomic Absorption Spectrometers 78

3.1.2 The Lambert-Beer Law in Atomic Absorption Spectrometry 78

3.1.3 Scale Expansion 81

3.1.4 Single-beam and Double-beam Instruments 82

3.1.5 Multi-channel Instruments 83

3.1.6 Modulation of the Signal 84

3.1.7 Readout Devices 85

3.1.8 Optimization of Operating Parameters 85

3.1.9 Automation 87

3.1.9.1 Sample Preparation 87

3.1.9.2 Sample Dilution 87

3.1.9.3 Sample Introduction 87

3.1.9.4 Multi-element Analysis 88

3.1.10 Fault Finding 88

3.1.10.1 Flame AAS 88

3.1.10.2 Electrothermal AAS 89

3.2 Flame Atomization 90

3.2.1 Flames 91

3.2.1.1 Combustion Flames 91

3.2.1.2 Diffusion Flame 94

3.2.2 Nebulizer-Burner Systems 94

3.2.2.1 Pneumatic Nebulizer 95

3.2.2.2 Spray Chambers 98

3.2.2.3 Ultrasonic Nebulizer 98

3.2.2.4 Direct Introduction of Solid Samples 99

3.2.2.5 Burners 100

3.2.3 Atomization Process in the Flame 101

3.2.4 Interferences in Flame Atomization 104

3.2.4.1 Chemical Interferences 104

3.2.4.2 Ionization Interferences 107

3.2.4.3 Physical Interferences 107

3.2.4.4 Spectral Interferences 108

3.3 Electrothermal Atomization 109

3.3.1 Graphite Furnace Atomizers 109

3.3.1.1 Stabilized Temperature Platform Furnace 113

3.3.1.2 Probe Atomization 117

3.3.2 Open Filament Atomizers 119

3.3.3 Vertical Crucible Furnace Atomizers 120

3.3.4 Graphite Cuvettes 121

3.3.4.1 Cuvette Material 121

3.3.4.2 Pyrolytically Coated Graphite Cuvettes 122

3.3.4.3 Totally Pyrographite Cuvettes 123

3.3.4.4 Graphite Cuvette Geometries 126

3.3.4.5 Platform Cuvettes 126

3.3.4.6 Ridged Cuvettes 128

3.3.5 Atomization Process 128

3.3.5.1 Drying 131

3.3.5.2 Thermal Pretreatment 131

3.3.5.3 Atomization 132

3.3.5.4 Platform Atomization 137

3.3.5.5 Probe Atomization 137

3.3.6 Analysis of Solid Samples 139

3.3.7 Matrix Modification 142

3.3.8 Interferences in Graphite Furnace Atomization 147

3.3.8.1 Physical Interferences 147

3.3.8.2 Chemical Interferences 148

3.4 Background Correction 149

3.4.1 Two Line Method 150

3.4.2 Continuum Source Method 150

3.4.2.1 Continuum Radiation Sources 152

3.4.2.2 Faults in Background Correction 152

3.4.3 Smith-Hieftje Method 155

3.4.4 Methods Achieving Zeeman Effect 157

3.4.4.1 Direct Zeeman AAS 157

3.4.4.2 Inverse Zeeman AAS 158

3.5 Special Methods 169

3.5.1 Slotted Tube Atom Trap 169

3.5.2 Hydride Generation Methods 170

3.5.2.1 Atomization of the Hydrides 172

3.5.2.2 Gas-Phase Interferences 173

3.5.3 Cold Vapour Technique 174

3.5.4 Semi-Flame Methods 177

3.5.4.1 Delves Cup 177

3.5.4.2 Sampling Boat 179

3.5.5 Indirect Methods 179

3.5.6 Molecular Absorption Spectrometry with Electrothermal Vaporization (ETV-MAS) 191

Chapter 4 Flame Atomic Emission Spectrometry 200

Chapter 5 Plasma Atomic Emission Spectrometry 202

5.1 Instrumentation for Plasma Atomic Emission Spectrometry 203

5.2 Plasma Sources 203

5.2.1 Inductively Coupled Plasmas 204

5.2.1.1 Types of Inductively Coupled Plasmas 205

5.2.1.2 Radio-Frequency Generators 207

5.2.2 Direct Current Plasmas 208

5.2.3 Microwave Plasmas 211

5.3 Sample Introduction 215

5.3.1 Solutions 215

5.3.1.1 Pneumatic Nebulization 215

5.3.1.2 Ultrasonic Nebulizers 216

5.3.1.3 Grid Nebulizer 217

5.3.1.4 Spray Chambers and Desolvation System 218

5.3.1.5 Nebulizers for Low Sample Volumes 220

5.3.2 Solid Samples 221

5.3.2.1 Direct Insertion of Samples 221

5.3.2.2 Methods that Convert Solid Samples into an Aerosol or Vapour 224

5.3.3 Gaseous Samples 227

5.3.3.1 Hydride Generation Method 227

5.3.3.2 Cold Vapour Method 231

5.4 Spectrometers 231

5.4.1 Spectrometers with the Paschen-Runge Mount 231

5.4.2 Echelle Spectrometers 233

5.4.3 Spectrometers with the Ebert and Czerny-Turner Mounts 241

5.4.4 Spectrometers with the Seya-Namioka Mounts 241

5.4.5 Double Monochromators 241

5.4.6 ICP Atomic Emission Fourier Transform Spectrometers 242

5.5 Interference Effects and Background Correction 244

5.5.1 Nebulization Interferences 245

5.5.2 Chemical Interferences 246

5.5.3 Ionization Interferences 246

5.5.4 Spectral Interferences 246

5.5.4.1 Spectral Line Coincidence 247

5.5.4.2 Overlap with Nearby Broadened Line Wing 248

5.5.4.3 Spectral Continuum and Stray Light 248

5.5.5 Background Correction 251

5.6 Analytical Features of an Argon ICP 253

5.6.1 Emission Lines Employed in ICP-AES 254

5.6.2 Optimization of Instrumental Parameters 255

Chapter 6 Inductively Coupled Plasma Mass Spectrometry 257

6.1 Instrumentation 257

6.2 Sample Introduction 260

6.2.1 Laser Ablation 261

6.2.2 Arc Nebulization 266

6.2.3 Electrothermal Vaporization (ETV) 266

6.3 Interference Effects 267

6.3.1 Signal Enhancement and Suppression 268

6.3.2 Spectral Interferences 269

6.3.2.1 Elimination of Spectral Interferences 270

Chapter 7 Atomic Fluorescence Spectrometry 276

7.1 The Relationship Between Fluorescence and Concentration 277

7.2 Instrumentation for Atomic Fluorescence Spectrometry 278

7.2.1 Radiation Sources 279

7.2.1.1 Hollow Cathode Lamps 279

7.2.1.2 EDLs 279

7.2.1.3 Lasers 280

7.2.1.4 Plasma 280

7.2.1.5 Xenon Arc Lamp 280

7.2.2 Atomizers 281

7.2.2.1 Flames 281

7.2.2.2 Plasma 281

7.2.2.3 Electrothermal Atomizers 282

7.2.2.4 Glow Discharge Chamber 282

7.2.3 Selection of the Wavelength 282

7.2.3.1 Non-dispersive Instruments 282

7.2.3.2 Dispersive Instruments 283

7.3 Interference Effects 283

7.4 Analytical Applications of AFS 284

Chapter 8 Sample Preparation 286

8.1 Sample Collection and Storage 286

8.2 Systematic Errors: Contamination and Adsorption 287

8.3 Sample Preparation Methods 291

8.3.1 Liquid Samples 294

8.3.1.1 Aqueous Solutions 294

8.3.1.2 Non-Aqueous Solutions 295

8.3.1.3 Emulsions 298

8.3.2 Solid Samples 299

8.3.2.1 Dry Ashing 300

8.3.2.2 Wet Digestion 300

8.3.2.3 Digestion in Closed Vessels (Pressure Digestion) 301

8.3.2.4 Fusion 304

8.3.2.5 Slurries 305

8.4 Separation and Preconcentration Methods 305

8.4.1 Liquid-Liquid Extraction 306

8.4.1.1 Extraction Systems 306

8.4.1.2 Standards and Blank Samples 310

8.4.1.3 Back Extraction 311

8.4.2 Ion Exchange 311

8.4.3 Solid Phase Extraction 311

8.4.4 Precipitation 313

8.4.5 Evaporation 313

Chapter 9 Hypheneted Techniques 314

9.1 Atomic Spectrometric Detectors 315

9.2 Separation Methods 317

9.2.1 Gas Chromatography 317

9.2.2 Liquid Chromatography 320

Chapter 10 Advantages and Mutual Comparison of Atomic Spectrometric Methods 324

10.1 Detection Limits 324

10.2 Atomic Absorption 324

10.3 Plasma Atomic Emission 326

10.4 Plasma Mass Spectrometry 328

10.5 Atomic Fluorescence 328

11.2 General Journals, Specialist Journals, Abstracts, and Reviews 330

11.2.1 General journals 330

11.2.2 Specialist Journals 330

11.2.3 Abstracts and Reviews 330.

Notes:

Includes bibliographical references and index.

Local Notes:

Acquired for the Penn Libraries with assistance from the Alumni and Friends Memorial Book Fund.

ISBN:

0854046240

OCLC:

57355538