Environmental Trace Analysis: Techniques and Applications -- Contents -- About the Author -- Preface -- Acknowledgements -- Acronyms and Abbreviations -- 1 Basic Laboratory Procedures -- 1.1 Introduction -- 1.2 Health and Safety Issues -- 1.3 Sample Handling: Solid Samples -- 1.4 Sample Handling: Liquid Samples -- 1.5 Sample Handling: Gases/Vapour Samples -- 1.6 Summary -- Further Reading -- 2 Investigative Approach for Environmental Analysis -- 2.1 Introduction -- 2.2 Recording of Practical Results -- 2.2.1 Useful Tips on Presenting Data in Tables -- 2.2.2 Useful Tips on Presenting Data in Graphical Form -- 2.2.3 Useful Tips for Templates for Presenting Data in Your Notebook -- 2.3 Significant Figures -- 2.4 Units -- 2.5 Summary -- Appendix -- Example Template A: Sample Collection -- Example Template B: Sample Treatment -- Example Template C: Sample Preparation for Inorganic Analysis -- Example Template D: Instrumental Analysis -- Example Template E: Sample Preparation for Organic Analysis -- Example Template F: Instrumental Analysis -- Further Reading -- 3 Principles of Quantitative Environmental Analysis -- 3.1 Introduction -- 3.2 Preparing Solutions for Quantitative Work -- 3.3 Calibration Graphs -- 3.4 Limits of Detection/Quantitation -- 3.5 Calculations: Dilution or Concentration Factors -- 3.6 Quality Assurance -- 3.6.1 Certified Reference Materials -- 3.7 Summary -- References -- Further Reading -- 4 Environmental Sampling -- 4.1 Introduction -- 4.2 Sampling Soil (and Sediments) -- 4.3 Sampling Water -- 4.4 Sampling Air -- 4.5 Summary -- Further Reading -- 5 Storage of Samples for Analysis -- 5.1 Introduction -- 5.2 Choice of Storage Container for Liquid Samples -- 5.3 Preservation Techniques for Liquid Samples -- 5.4 Storage and Preservation of Solid Samples -- 5.5 Storage and Preservation of Gaseous Samples -- 5.6 Summary.

Further Reading -- 6 Preparation of Environmental Solid Samples for Inorganic Analysis -- 6.1 Introduction -- 6.2 Decomposition Techniques -- 6.3 Selective Extraction Methods -- 6.3.1 Single Extraction Methods -- 6.3.2 Sequential Extraction Method -- 6.3.3 Chemometric Identification of Substrates and Element Distributions (CISED) Method -- 6.4 Physiologically-Based Extraction Test or In Vitro Gastrointestinal Extraction -- 6.4.1 Procedure for Gastric Extraction -- 6.4.2 Procedure for Gastric + Intestinal Extraction -- 6.5 Earthworms -- 6.5.1 Procedure for Earthworm Bioaccumulation Studies (Sandoval et al., 2001) -- 6.6 Summary -- Appendix A: Extraction Reagents for Single Extraction Methods -- Appendix B: Extraction Reagents for Sequential Extraction Method -- Appendix C: Extraction Reagents for In Vitro Gastrointestinal Extraction Using the Unified Bioaccessibility Method (and the FOREhST Method) -- References -- Further Reading -- 7 Preparation of Environmental Liquid Samples for Inorganic Analysis -- 7.1 Introduction -- 7.2 Liquid-Liquid Extraction of Metals -- 7.2.1 Procedure for APDC Extraction into MIBK -- 7.3 Ion Exchange -- 7.3.1 Chelation Ion Exchange -- 7.3.2 Procedure for Batch Ion Exchange Extraction -- 7.4 Co-precipitation -- 7.5 Summary -- References -- Further Reading -- 8 Preparation of Environmental Solid Samples for Organic Analysis -- 8.1 Introduction -- 8.2 Liquid-Solid Extraction -- 8.2.1 Soxhlet Extraction -- 8.2.2 Soxtec Extraction -- 8.2.3 Shake Flask Extraction -- 8.2.4 Ultrasonic Extraction -- 8.3 Pressurised Fluid Extraction -- 8.3.1 Instrumentation -- 8.3.2 In Situ Clean-up or Selective PFE -- 8.3.3 Procedure for Pressurised Fluid Extraction -- 8.4 Microwave-Assisted Extraction -- 8.4.1 Instrumentation -- 8.4.2 Procedure for Microwave-Assisted Extraction -- 8.5 Supercritical Fluid Extraction -- 8.5.1 Instrumentation.

8.5.2 Procedure for Supercritical Fluid Extraction -- 8.6 Matrix Solid Phase Dispersion -- 8.7 Physiologically-Based Extraction Test or In Vitro Gastrointestinal Extraction -- 8.7.1 Procedure for Gastric + Intestinal Extraction -- 8.8 A Comparison of Extraction Techniques -- 8.9 Summary -- Appendix A: Suppliers of Instrumental Techniques -- Appendix B: Extraction Reagents for In Vitro Gastrointestinal Extraction Using the FOREhST Method (and the Unified Bioaccessibility Method) -- Preparation of Simulated Saliva Fluid -- Preparation of Simulated Gastric Fluid -- Preparation of Simulated Duodenal Fluid -- Preparation of Simulated Bile Fluid -- References -- Further Reading -- 9 Preparation of Environmental Liquid Samples for Organic Analysis -- 9.1 Introduction -- 9.2 Liquid-Liquid Extraction -- 9.2.1 Procedure for Discontinuous Extraction -- 9.2.2 Procedure for Continuous Extraction -- 9.2.3 An Issue in Liquid-Liquid Extraction -- 9.3 Solid Phase Extraction -- 9.3.1 Procedure for Solid Phase Extraction -- 9.4 Purge and Trap Extraction -- 9.4.1 Procedure for Purge and Trap Extraction -- 9.5 Headspace Extraction -- 9.5.1 Procedures for Headspace Sampling -- 9.5.2 Main Issues in Static Headspace (SHS) Analysis -- 9.5.3 Main Issues in Dynamic Headspace (DHS) Analysis -- 9.6 Solid Phase Microextraction -- 9.6.1 Procedure for Solid Phase Microextraction -- 9.6.2 Main Issues in Solid Phase Microextraction -- 9.7 Stir-Bar Sorptive Extraction -- 9.7.1 Main Issues in Stir-Bar Sorptive Extraction -- 9.8 Microextraction in a Packed Syringe -- 9.8.1 Procedure for Microextraction in a Packed Syringe -- 9.8.2 Main Issues in Microextraction in a Packed Syringe -- 9.9 Liquid Phase Microextraction -- 9.9.1 Main Issues in Single Drop Microextraction -- 9.10 Membrane Extraction -- 9.10.1 Semi-Permeable Membrane -- 9.10.2 Polar Organic Chemical Integrative Sampler.

9.10.3 Chemcatcher -- 9.10.4 Ceramic Dosimeter -- 9.10.5 Membrane Enclosed-Sorptive Coating -- 9.11 A Comparison of Extraction Techniques -- 9.12 Summary -- References -- Further Reading -- 10 Preparation of Environmental Air Samples for Organic Analysis -- 10.1 Introduction -- 10.2 Thermal Desorption -- 10.2.1 Procedure for Thermal Desorption -- 10.3 Summary -- Further Reading -- 11 Pre-concentration and Clean-up Procedures for Organic Sample Extracts -- 11.1 Introduction -- 11.2 Methods for Solvent Evaporation -- 11.3 Sample Extract Clean-up Procedures -- 11.3.1 Column Chromatography -- 11.3.2 Acid-Alkaline Partition -- 11.3.3 Acetonitrile-Hexane Partition -- 11.3.4 Sulfur Clean-up -- 11.3.5 Alkaline Decomposition -- 11.4 Summary -- Further Reading -- 12 Instrumental Techniques for Environmental Trace Analysis -- 12.1 Introduction -- 12.2 Environmental Inorganic Analysis -- 12.2.1 Atomic Spectroscopy -- 12.2.2 Inorganic Mass Spectrometry -- 12.2.3 X-ray Fluorescence Spectroscopy -- 12.2.4 Other Techniques for Environmental Inorganic Analysis -- 12.3 Environmental Organic Analysis -- 12.3.1 Gas Chromatography -- 12.3.2 High Performance Liquid Chromatography -- 12.4 Other Techniques for Environmental Organic Analysis -- 12.5 Portable Techniques for Field Measurements -- 12.6 Summary -- Further Reading -- Portable Techniques -- 13 Selected Case Studies -- 13.1 Introduction -- 13.2 Total Analysis of Metals from Soils -- 13.3 Single Extraction of Metals from Soils -- 13.4 Sequential Extraction of Metals from Soils -- 13.5 Oral Bioaccessibility Testing of Metals from Soils -- 13.6 Pressurised Fluid Extraction of Organic Compounds from Soils -- 13.7 Solid Phase Extraction of Organic Compounds from Liquid Samples -- 13.8 Headspace Solid Phase Microextraction of Organic Compounds -- 13.9 Dynamic Headspace Analysis of Organic Compounds.

13.10 An Environmental Case Study: From Site to Analysis to Data Interpretation and Contextualisation -- 13.10.1 Preliminary Risk Assessment -- 13.10.2 Generic Quantitative Risk Assessment (GQRA) (Stanger, 2004) -- 13.10.3 Detailed Quantitative Risk Assessment (DQRA) -- 13.10.4 Remediation -- 13.11 Summary -- References -- 14 Some Numerical Worked Examples -- 14.1 Introduction -- Index.