Environmental Trace Analysis

About the Author xv
Preface xvii
Acknowledgements xix
Acronyms and Abbreviations xxi
1 Basic Laboratory Procedures 1
1.1 Introduction 1
1.2 Health and Safety Issues 2
1.3 Sample Handling: Solid Samples 4
1.4 Sample Handling: Liquid Samples 4
1.5 Sample Handling: Gases/Vapour Samples 5
1.6 Summary 5
2 Investigative Approach for Environmental Analysis 7
2.1 Introduction 7
2.2 Recording of Practical Results 7
2.3 Significant Figures 9
2.4 Units 12
2.5 Summary 13
3 Principles of Quantitative Environmental Analysis 21
3.1 Introduction 21
3.2 Preparing Solutions for Quantitative Work 23
3.3 Calibration Graphs 24
3.4 Limits of Detection/Quantitation 27
3.5 Calculations: Dilution or Concentration Factors 27
3.6 Quality Assurance 29
3.7 Summary 36
4 Environmental Sampling 37
4.1 Introduction 37
4.2 Sampling Soil (and Sediments) 39
4.3 Sampling Water 40
4.4 Sampling Air 42
4.5 Summary 44
5 Storage of Samples for Analysis 45
5.1 Introduction 45
5.2 Choice of Storage Container for Liquid Samples 45
5.3 Preservation Techniques for Liquid Samples 47
5.4 Storage and Preservation of Solid Samples 48
5.5 Storage and Preservation of Gaseous Samples 48
5.6 Summary 50
6 Preparation of Environmental Solid Samples for Inorganic Analysis 51
6.1 Introduction 51
6.2 Decomposition Techniques 53
6.3 Selective Extraction Methods 64
6.4 Physiologically-Based Extraction Test or In Vitro Gastrointestinal Extraction 70
6.5 Earthworms 72
6.6 Summary 75
7 Preparation of Environmental Liquid Samples for Inorganic Analysis 81
7.1 Introduction 81
7.2 Liquid-Liquid Extraction of Metals 82
7.3 Ion Exchange 83
7.4 Co-precipitation 84
7.5 Summary 84
8 Preparation of Environmental Solid Samples for Organic Analysis 85
8.1 Introduction 85
8.2 Liquid-Solid Extraction 85
8.3 Pressurised Fluid Extraction 91
8.4 Microwave-Assisted Extraction 100
8.5 Supercritical Fluid Extraction 103
8.6 Matrix Solid Phase Dispersion 107
8.7 Physiologically-Based Extraction Test or In Vitro Gastrointestinal Extraction 108
8.8 A Comparison of Extraction Techniques 109
8.9 Summary 112
9 Preparation of Environmental Liquid Samples for Organic Analysis 115
9.1 Introduction 115
9.2 Liquid-Liquid Extraction 116
9.3 Solid Phase Extraction 120
9.4 Purge and Trap Extraction 127
9.5 Headspace Extraction 128
9.6 Solid Phase Microextraction 132
9.7 Stir-Bar Sorptive Extraction 135
9.8 Microextraction in a Packed Syringe 137
9.9 Liquid Phase Microextraction 139
9.10 Membrane Extraction 140
9.11 A Comparison of Extraction Techniques 143
9.12 Summary 143
10 Preparation of Environmental Air Samples for Organic Analysis 145
10.1 Introduction 145
10.2 Thermal Desorption 147
10.3 Summary 148
11 Pre-concentration and Clean-up Procedures for Organic Sample Extracts 149
11.1 Introduction 149
11.2 Methods for Solvent Evaporation 149
11.3 Sample Extract Clean-up Procedures 151
11.4 Summary 154
12 Instrumental Techniques for Environmental Trace Analysis 157
12.1 Introduction 157
12.2 Environmental Inorganic Analysis 157
12.3 Environmental Organic Analysis 176
12.4 Other Techniques for Environmental Organic Analysis 188
12.5 Portable Techniques for Field Measurements 189
12.6 Summary 195
13 Selected Case Studies 197
13.4 Sequential Extraction of Metals from Soils 201
13.5 Oral Bioaccessibility Testing of Metals from Soils 204
13.6 Pressurised Fluid Extraction of Organic Compounds from Soils 206
13.7 Solid Phase Extraction of Organic Compounds from Liquid Samples 210
13.8 Headspace Solid Phase Microextraction of Organic Compounds 211
13.9 Dynamic Headspace Analysis of Organic Compounds 215
13.10 An Environmental Case Study: From Site to Analysis to Data Interpretation and Contextualisation 217
13.11 Summary 232
References 237
14 Some Numerical Worked Examples 239
14.1 Introduction 239
Index 251