Environmental Trace Analysis - Techniques and Applications

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