Environmental Trace Analysis

Professor John Dean, Professor of Analytical and Environmental Science, Northumbria University, UKFellow of the Royal Society of Chemistry (FRSC); Chartered Chemist (C.Chem.); Chartered Scientist (C.Sci.); Registered Analytical ChemistJohn Dean's recent research work has focused on (a) the application of the physiologically-based extraction test to assess environmental health risk from metals and polycyclic aromatic hydrocarbons in contaminated land studies, (b) development of new high performance liquid chromatographic approaches for environmental and pharmaceutical compounds, and, (c) development of novel gas chromatographic approaches as a diagnostic tool for bacterial detection/identification.

• About the Author xvPreface xviiAcknowledgements xixAcronyms and Abbreviations xxi1 Basic Laboratory Procedures 11.1 Introduction 11.2 Health and Safety Issues 21.3 Sample Handling: Solid Samples 41.4 Sample Handling: Liquid Samples 41.5 Sample Handling: Gases/Vapour Samples 51.6 Summary 52 Investigative Approach for Environmental Analysis 72.1 Introduction 72.2 Recording of Practical Results 72.3 Significant Figures 92.4 Units 122.5 Summary 133 Principles of Quantitative Environmental Analysis 213.1 Introduction 213.2 Preparing Solutions for Quantitative Work 233.3 Calibration Graphs 243.4 Limits of Detection/Quantitation 273.5 Calculations: Dilution or Concentration Factors 273.6 Quality Assurance 293.7 Summary 364 Environmental Sampling 374.1 Introduction 374.2 Sampling Soil (and Sediments) 394.3 Sampling Water 404.4 Sampling Air 424.5 Summary 445 Storage of Samples for Analysis 455.1 Introduction 455.2 Choice of Storage Container for Liquid Samples 455.3 Preservation Techniques for Liquid Samples 475.4 Storage and Preservation of Solid Samples 485.5 Storage and Preservation of Gaseous Samples 485.6 Summary 506 Preparation of Environmental Solid Samples for Inorganic Analysis 516.1 Introduction 516.2 Decomposition Techniques 536.3 Selective Extraction Methods 646.4 Physiologically-Based Extraction Test or In Vitro Gastrointestinal Extraction 706.5 Earthworms 726.6 Summary 757 Preparation of Environmental Liquid Samples for Inorganic Analysis 817.1 Introduction 817.2 Liquid-Liquid Extraction of Metals 827.3 Ion Exchange 837.4 Co-precipitation 847.5 Summary 848 Preparation of Environmental Solid Samples for Organic Analysis 858.1 Introduction 858.2 Liquid-Solid Extraction 858.3 Pressurised Fluid Extraction 918.4 Microwave-Assisted Extraction 1008.5 Supercritical Fluid Extraction 1038.6 Matrix Solid Phase Dispersion 1078.7 Physiologically-Based Extraction Test or In Vitro Gastrointestinal Extraction 1088.8 A Comparison of Extraction Techniques 1098.9 Summary 1129 Preparation of Environmental Liquid Samples for Organic Analysis 1159.1 Introduction 1159.2 Liquid–Liquid Extraction 1169.3 Solid Phase Extraction 1209.4 Purge and Trap Extraction 1279.5 Headspace Extraction 1289.6 Solid Phase Microextraction 1329.7 Stir-Bar Sorptive Extraction 1359.8 Microextraction in a Packed Syringe 1379.9 Liquid Phase Microextraction 1399.10 Membrane Extraction 1409.11 A Comparison of Extraction Techniques 1439.12 Summary 14310 Preparation of Environmental Air Samples for Organic Analysis 14510.1 Introduction 14510.2 Thermal Desorption 14710.3 Summary 14811 Pre-concentration and Clean-up Procedures for Organic Sample Extracts 14911.1 Introduction 14911.2 Methods for Solvent Evaporation 14911.3 Sample Extract Clean-up Procedures 15111.4 Summary 15412 Instrumental Techniques for Environmental Trace Analysis 15712.1 Introduction 15712.2 Environmental Inorganic Analysis 15712.3 Environmental Organic Analysis 17612.4 Other Techniques for Environmental Organic Analysis 18812.5 Portable Techniques for Field Measurements 18912.6 Summary 19513 Selected Case Studies 19713.4 Sequential Extraction of Metals from Soils 20113.5 Oral Bioaccessibility Testing of Metals from Soils 20413.6 Pressurised Fluid Extraction of Organic Compounds from Soils 20613.7 Solid Phase Extraction of Organic Compounds from Liquid Samples 21013.8 Headspace Solid Phase Microextraction of Organic Compounds 21113.9 Dynamic Headspace Analysis of Organic Compounds 21513.10 An Environmental Case Study: From Site to Analysis to Data Interpretation and Contextualisation 21713.11 Summary 232References 23714 Some Numerical Worked Examples 23914.1 Introduction 239Index 251