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Extraction Methods for Environmental Analysis
by
JOHN R. DEAN
by
JOHN R. DEAN
By
Publisher: Wiley
Number Of Pages: 240
Publication Date: 1998-08-31
ISBN-10 / ASIN: 0471982873
ISBN-13 / EAN: 9780471982876
Product Description
Extraction Methods for Environmental Analysis is the first book to bring together all the extraction techniques used for analysis of liquid and solid environmental samples, including solid phase extraction and micro-extraction, supercritical fluid extraction, microwave-assisted extraction and accelerated solvent extraction. The book is divided into two sections - solid sample preparation and liquid sample preparation - to facilitate access, and each section starts with a summary of methods available. The techniques are compared and contrasted by means of 70 bar charts, all in two colours, and 32 tables. Relative merits of the techniques are discussed to enable the user to select the most appropriate technique for their sample and method of analysis. Extraction Methods for Environmental Analysis is essential reading for anyone involved in environmental analysis
Extraction Methods for Environmental Analysis is the first book to bring together all the extraction techniques used for analysis of liquid and solid environmental samples, including solid phase extraction and micro-extraction, supercritical fluid extraction, microwave-assisted extraction and accelerated solvent extraction. The book is divided into two sections - solid sample preparation and liquid sample preparation - to facilitate access, and each section starts with a summary of methods available. The techniques are compared and contrasted by means of 70 bar charts, all in two colours, and 32 tables. Relative merits of the techniques are discussed to enable the user to select the most appropriate technique for their sample and method of analysis. Extraction Methods for Environmental Analysis is essential reading for anyone involved in environmental analysis
CONTENTS
Environmental Analysis
1. 1 Introduction 1
1.2 Sampling Strategies 3
1.2.1 Sampling Water Matrices 4
1.2.2 Sampling Soils and Sludges 4
1.3 Storage of Samples 5
1.4 Brief Introduction to Practical Chromatographic Analysis 6
1.5 Quality Assurance in Environmental Analysis 10
References 11
Bibliography 11
Part I: Aqueous Samples
2.Aqueous Sample Preparation
2.1 Environmental Case Study: Pesticides 15
2.1.1 Environmental Fate and Behaviour of Pesticides 18
References 21
3.Classical Approaches for the Extraction of Analytes from Aqueous
Samples
3.1 Liquid-Liquid Extraction 23
3.1.1 Theory of Liquid-Liquid Extraction 23
3.1.2 Solvent Extraction 25
3.1.3 Solvent Evaporation Methods 27
3.2 Purge and Trap for Volatile Organics 33
References 34
4.Solid Phase Extraction
4.1 Types of SPE Media 35
4.2 Cartridge or Disk Format 36
4.3 Method of SPE Operation 40
4.4 Solvent Selection 42
4.5 Factors Affecting SPE 43
4.6 Selected Methods of Analysis for SPE 43
4.7 Automated and On -line SPE 46
4.8 Selected Applications of Automated On-line SPE 48
References 61
5.Solid Phase Microextraction
5.1 Theoretical Considerations 65
5.2 Experimental 66
5.3 Methods of Analysis: SPME-GC 67
5.3.1 Volatile Organics in Water: Direct Extraction 67
5.3.2 Volatile Organics in Water: Headspace Concentration 70
5.3.3 Pesticides from Aqueous Samples 72
5.3.4 Phenols 75
5.3.5 Analysis of Analytes from Solid Matrices 78
5.4 Methods of Analysis: SPME-HPLC 83
5.5 Miscellaneous Applications 84
5.5.1 Characterisation of Alcoholic Beverages 84
5.5.2 Analysis of Human Breath 86
5.5.3 Analysis of Cigarette Smoke Condensate 88
5.5.4 Headspace SPME of Cinnamon 88
5.5.5 Tetraethylead and Inorganic Lead in Water 90
5.5.6 Solid Phase Microextraction-Electrodeposition Device 90
5.5.7 Analysis of Polar Analytes using Derivatisation/SPME 90
References 94
Bibliography 94
Part II: Solid Samples
6.Solid Sample Preparation99
6.1 Introduction 101
References 106
7.Liquid-Solid Extraction107
7.1 Introduction 107
7.2 Experimental 107
7.3 Selected Methods of Analysis 109
7.3.1 Soxhlet 110
7.3.2 Soxtec (Automated Soxhlet) 110
7.3.3 Shake-Flask 112
7.3.4 Shake-Flask versus Sonication 114
7.3.5 Shake-Flask versus Reflux (Soxhlet) 117
7.3.6 Sonication versus Soxhlet 118
7.3.7 Other Approaches 119
References 121
8.Supercritical Fluid Extraction
8.1 Definition of a Supercritical Fluid 125
8.2 Instrumentation for Supercritical Fluid Extraction 126
8.3 Methods of Analysis: Extraction from Solid Samples 129
8.3.1 Polycyclic Aromatic Hydrocarbons 130
8.3.2 Polychlorinated Biphenyls 134
8.3.3 Phenols 139
8.3.4 Pesticides 146
8.4 Methods of Analysis: Extraction from Aqueous Samples 153
8.4.1 Direct Extraction of Analytes from Aqueous Samples 154
8.4.2 Use of a Combined SPE-SFE Approach 155
8.5 Recommendations for SFE 156
8.5.1 Selection of Initial Extraction Conditions 158
8.5.2 Preliminary Extractions of Representative Samples 158
8.5.3 Determination of Collection Efficiencies 160
8.5.4 Determine Extraction Efficiency 161
8.5.5 Optimisation of SFE Conditions 161
References 162
Bibliography 163
9.Microwave-Assisted Extraction165
9.1 Theoretical Considerations 165
9.2 Instrumentation 167
9.3 Methods of Analysis: Extraction from Solids 169
9.3.1 Polycyclic Aromatic Hydrocarbons 170
9.3.2 Pesticides 172
9.3.3 Herbicides 175
9.3.4 Phenols 175
9.3.5 Polychlorinated Biphenyls 176
9.3.6 Phthalate Esters 176
9.3.7 Organometallics 177
9.4 Methods of Analysis: Extraction from Water 179
9.5 Gas-Phase Microwave-Assisted Extraction 181
9.6 Comparison with other Extraction Techniques 181
9.6.1 Polycyclic Aromatic Hydrocarbons 184
9.6.2 Organochlorine Pesticides 184
9.6.3 Phenols 184
9.6.4 Phthalate Esters 186
9.7 Recommendations for MAE 186
References 187
Appendix A 188
10.Accelerated Solvent Extraction189
10.1 Theoretical Considerations 189
10.1.1 Solubility and Mass Transfer Effects 189
10.1.2 Disruption of Surface Equilibria 189
10.2 Instrumentation 190
10.3 Applications 191
10.3.1 Polycyclic Aromatic Hydrocarbons 191
10.3.2 Polychlorinated Biphenyls 197
10.3.3 Dioxins and Furans 198
10.3.4 Pesticides 199
10.3.5 Phenols 203
10.4 Recommendations for ASE 207
References 209
11. Comparison of Extraction Methods 211
11.1 Future Developments in Sample Preparation 211
References 216
General Index 217
Chemical Index 221
Environmental Analysis
1. 1 Introduction 1
1.2 Sampling Strategies 3
1.2.1 Sampling Water Matrices 4
1.2.2 Sampling Soils and Sludges 4
1.3 Storage of Samples 5
1.4 Brief Introduction to Practical Chromatographic Analysis 6
1.5 Quality Assurance in Environmental Analysis 10
References 11
Bibliography 11
Part I: Aqueous Samples
2.Aqueous Sample Preparation
2.1 Environmental Case Study: Pesticides 15
2.1.1 Environmental Fate and Behaviour of Pesticides 18
References 21
3.Classical Approaches for the Extraction of Analytes from Aqueous
Samples
3.1 Liquid-Liquid Extraction 23
3.1.1 Theory of Liquid-Liquid Extraction 23
3.1.2 Solvent Extraction 25
3.1.3 Solvent Evaporation Methods 27
3.2 Purge and Trap for Volatile Organics 33
References 34
4.Solid Phase Extraction
4.1 Types of SPE Media 35
4.2 Cartridge or Disk Format 36
4.3 Method of SPE Operation 40
4.4 Solvent Selection 42
4.5 Factors Affecting SPE 43
4.6 Selected Methods of Analysis for SPE 43
4.7 Automated and On -line SPE 46
4.8 Selected Applications of Automated On-line SPE 48
References 61
5.Solid Phase Microextraction
5.1 Theoretical Considerations 65
5.2 Experimental 66
5.3 Methods of Analysis: SPME-GC 67
5.3.1 Volatile Organics in Water: Direct Extraction 67
5.3.2 Volatile Organics in Water: Headspace Concentration 70
5.3.3 Pesticides from Aqueous Samples 72
5.3.4 Phenols 75
5.3.5 Analysis of Analytes from Solid Matrices 78
5.4 Methods of Analysis: SPME-HPLC 83
5.5 Miscellaneous Applications 84
5.5.1 Characterisation of Alcoholic Beverages 84
5.5.2 Analysis of Human Breath 86
5.5.3 Analysis of Cigarette Smoke Condensate 88
5.5.4 Headspace SPME of Cinnamon 88
5.5.5 Tetraethylead and Inorganic Lead in Water 90
5.5.6 Solid Phase Microextraction-Electrodeposition Device 90
5.5.7 Analysis of Polar Analytes using Derivatisation/SPME 90
References 94
Bibliography 94
Part II: Solid Samples
6.Solid Sample Preparation99
6.1 Introduction 101
References 106
7.Liquid-Solid Extraction107
7.1 Introduction 107
7.2 Experimental 107
7.3 Selected Methods of Analysis 109
7.3.1 Soxhlet 110
7.3.2 Soxtec (Automated Soxhlet) 110
7.3.3 Shake-Flask 112
7.3.4 Shake-Flask versus Sonication 114
7.3.5 Shake-Flask versus Reflux (Soxhlet) 117
7.3.6 Sonication versus Soxhlet 118
7.3.7 Other Approaches 119
References 121
8.Supercritical Fluid Extraction
8.1 Definition of a Supercritical Fluid 125
8.2 Instrumentation for Supercritical Fluid Extraction 126
8.3 Methods of Analysis: Extraction from Solid Samples 129
8.3.1 Polycyclic Aromatic Hydrocarbons 130
8.3.2 Polychlorinated Biphenyls 134
8.3.3 Phenols 139
8.3.4 Pesticides 146
8.4 Methods of Analysis: Extraction from Aqueous Samples 153
8.4.1 Direct Extraction of Analytes from Aqueous Samples 154
8.4.2 Use of a Combined SPE-SFE Approach 155
8.5 Recommendations for SFE 156
8.5.1 Selection of Initial Extraction Conditions 158
8.5.2 Preliminary Extractions of Representative Samples 158
8.5.3 Determination of Collection Efficiencies 160
8.5.4 Determine Extraction Efficiency 161
8.5.5 Optimisation of SFE Conditions 161
References 162
Bibliography 163
9.Microwave-Assisted Extraction165
9.1 Theoretical Considerations 165
9.2 Instrumentation 167
9.3 Methods of Analysis: Extraction from Solids 169
9.3.1 Polycyclic Aromatic Hydrocarbons 170
9.3.2 Pesticides 172
9.3.3 Herbicides 175
9.3.4 Phenols 175
9.3.5 Polychlorinated Biphenyls 176
9.3.6 Phthalate Esters 176
9.3.7 Organometallics 177
9.4 Methods of Analysis: Extraction from Water 179
9.5 Gas-Phase Microwave-Assisted Extraction 181
9.6 Comparison with other Extraction Techniques 181
9.6.1 Polycyclic Aromatic Hydrocarbons 184
9.6.2 Organochlorine Pesticides 184
9.6.3 Phenols 184
9.6.4 Phthalate Esters 186
9.7 Recommendations for MAE 186
References 187
Appendix A 188
10.Accelerated Solvent Extraction189
10.1 Theoretical Considerations 189
10.1.1 Solubility and Mass Transfer Effects 189
10.1.2 Disruption of Surface Equilibria 189
10.2 Instrumentation 190
10.3 Applications 191
10.3.1 Polycyclic Aromatic Hydrocarbons 191
10.3.2 Polychlorinated Biphenyls 197
10.3.3 Dioxins and Furans 198
10.3.4 Pesticides 199
10.3.5 Phenols 203
10.4 Recommendations for ASE 207
References 209
11. Comparison of Extraction Methods 211
11.1 Future Developments in Sample Preparation 211
References 216
General Index 217
Chemical Index 221
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