Title Environmental trace analysis : techniques and applications / John R. Dean

Published Chichester, West Sussex, United Kingdom : Wiley, 2014

Table of Contents
	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
	Further Reading					5
2.	Investigative Approach for Environmental Analysis					7
2.1.	Introduction					7
2.2.	Recording of Practical Results					7
2.2.1.	Useful Tips on Presenting Data in Tables					8
2.2.2.	Useful Tips on Presenting Data in Graphical Form					9
2.2.3.	Useful Tips for Templates for Presenting Data in Your Notebook					9
2.3.	Significant Figures					9
2.4.	Units					12
2.5.	Summary					13
	Appendix					14
Example Template A	Sample Collection					14
Example Template B	Sample Treatment					14
Example Template C	Sample Preparation for Inorganic Analysis					15
Example Template D	Instrumental Analysis					17
Example Template E	Sample Preparation for Organic Analysis					18
Example Template F	Instrumental Analysis					20
	Further Reading					20
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
3.6.1.	Certified Reference Materials					30
3.7.	Summary					36
	References					36
	Further Reading					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
	Further Reading					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
	Further Reading					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
6.3.1.	Single Extraction Methods					64
6.3.2.	Sequential Extraction Method					67
6.3.3.	Chemometric Identification of Substrates and Element Distributions (CISED) Method					69
6.4.	Physiologically-Based Extraction Test or In Vitro Gastrointestinal Extraction					70
6.4.1.	Procedure for Gastric Extraction					71
6.4.2.	Procedure for Gastric + Intestinal Extraction					72
6.5.	Earthworms					72
6.5.1.	Procedure for Earthworm Bioaccumulation Studies (Sandoval et al., 2001)					74
6.6.	Summary					75
Appendix A	Extraction Reagents for Single Extraction Methods					75
Appendix B	Extraction Reagents for Sequential Extraction Method					77
Appendix C	Extraction Reagents for In Vitro Gastrointestinal Extraction Using the Unified Bioaccessibility Method (and the FOREhST Method)					77
	References					79
	Further Reading					80
7.	Preparation of Environmental Liquid Samples for Inorganic Analysis					81
7.1.	Introduction					81
7.2.	Liquid-Liquid Extraction of Metals					82
7.2.1.	Procedure for APDC Extraction into MIBK					82
7.3.	Ion Exchange					83
7.3.1.	Chelation Ion Exchange					83
7.3.2.	Procedure for Batch Ion Exchange Extraction					83
7.4.	Co-precipitation					84
7.5.	Summary					84
	References					84
	Further Reading					84
8.	Preparation of Environmental Solid Samples for Organic Analysis					85
8.1.	Introduction					85
8.2.	Liquid-Solid Extraction					85
8.2.1.	Soxhlet Extraction					86
8.2.2.	Soxtec Extraction					87
8.2.3.	Shake Flask Extraction					89
8.2.4.	Ultrasonic Extraction					90
8.3.	Pressurised Fluid Extraction					91
8.3.1.	Instrumentation					91
8.3.2.	In Situ Clean-up or Selective PFE					97
8.3.3.	Procedure for Pressurised Fluid Extraction					99
8.4.	Micro wave-Assisted Extraction					100
8.4.1.	Instrumentation					100
8.4.2.	Procedure for Microwave-Assisted Extraction					103
8.5.	Supercritical Fluid Extraction					103
8.5.1.	Instrumentation					105
8.5.2.	Procedure for Supercritical Fluid Extraction					106
8.6.	Matrix Solid Phase Dispersion					107
8.7.	Physiologically-Based Extraction Test or In Vitro Gastrointestinal Extraction					108
8.7.1.	Procedure for Gastric + Intestinal Extraction					109
8.8.	A Comparison of Extraction Techniques					109
8.9.	Summary					112
Appendix A	Suppliers of Instrumental Techniques					112
Appendix B	Extraction Reagents for In Vitro Gastrointestinal Extraction Using the FOREhST Method (and the Unified Bioaccessibility Method)					112
	Preparation of Simulated Saliva Fluid					112
	Preparation of Simulated Gastric Fluid					113
	Preparation of Simulated Duodenal Fluid					113
	Preparation of Simulated Bile Fluid					114
	References					114
	Further Reading					114
9.	Preparation of Environmental Liquid Samples for Organic Analysis					115
9.1.	Introduction					115
9.2.	Liquid-Liquid Extraction					116
9.2.1.	Procedure for Discontinuous Extraction					117
9.2.2.	Procedure for Continuous Extraction					119
9.2.3.	An Issue in Liquid-Liquid Extraction					119
9.3.	Solid Phase Extraction					120
9.3.1.	Procedure for Solid Phase Extraction					127
9.4.	Purge and Trap Extraction					127
9.4.1.	Procedure for Purge and Trap Extraction					127
9.5.	Headspace Extraction					128
9.5.1.	Procedures for Headspace Sampling					131
9.5.2.	Main Issues in Static Headspace (SHS) Analysis					131
9.5.3.	Main Issues in Dynamic Headspace (DHS) Analysis					132
9.6.	Solid Phase Microextraction					132
9.6.1.	Procedure for Solid Phase Microextraction					134
9.6.2.	Main Issues in Solid Phase Microextraction					135
9.7.	Stir-Bar Sorptive Extraction					135
9.7.1.	Main Issues in Stir-Bar Sorptive Extraction					136
9.8.	Microextraction in a Packed Syringe					137
9.8.1.	Procedure for Microextraction in a Packed Syringe					137
9.8.2.	Main Issues in Microextraction in a Packed Syringe					138
9.9.	Liquid Phase Microextraction					139
9.9.1.	Main Issues in Single Drop Microextraction					140
9.10.	Membrane Extraction					140
9.10.1.	Semi-Permeable Membrane					140
9.10.2.	Polar Organic Chemical Integrative Sampler					141
9.10.3.	Chemcatcher					141
9.10.4.	Ceramic Dosimeter					143
9.10.5.	Membrane Enclosed-Sorptive Coating					143
9.11.	A Comparison of Extraction Techniques					143
9.12.	Summary					143
	References					143
	Further Reading					144
10.	Preparation of Environmental Air Samples for Organic Analysis					145
10.1.	Introduction					145
10.2.	Thermal Desorption					147
10.2.1.	Procedure for Thermal Desorption					148
10.3.	Summary					148
	Further Reading					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
11.3.1.	Column Chromatography					152
11.3.2.	Acid-Alkaline Partition					153
11.3.3.	Acetonitrile-Hexane Partition					154
11.3.4.	Sulfur Clean-up					154
11.3.5.	Alkaline Decomposition					154
11.4.	Summary					154
	Further Reading					155
12.	Instrumental Techniques for Environmental Trace Analysis					157
12.1.	Introduction					157
12.2.	Environmental Inorganic Analysis					157
12.2.1.	Atomic Spectroscopy					157
12.2.2.	Inorganic Mass Spectrometry					168
12.2.3.	X-ray Fluorescence Spectroscopy					173
12.2.4.	Other Techniques for Environmental Inorganic Analysis					175
12.3.	Environmental Organic Analysis					176
12.3.1.	Gas Chromatography					176
12.3.2.	High Performance Liquid Chromatography					182
12.4.	Other Techniques for Environmental Organic Analysis					188
12.5.	Portable Techniques for Field Measurements					189
12.6.	Summary					195
	Further Reading					195
	Portable Techniques					196
13.	Selected Case Studies					197
13.1.	Introduction					197
13.2.	Total Analysis of Metals from Soils					197
13.3.	Single Extraction of Metals from Soils					199
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
13.10.1.	Preliminary Risk Assessment					219
13.10.2.	Generic Quantitative Risk Assessment (GQRA) (Stanger, 2004)					225
13.10.3.	Detailed Quantitative Risk Assessment (DQRA)					231
13.10.4.	Remediation					232
13.11.	Summary					232
	References					237
14.	Some Numerical Worked Examples					239
14.1.	Introduction					239
	Index					251

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Description 1 online resource Summary "The book covers all aspects of environmental trace analysis from sampling through to preparation of the sample to the analytical techniques used to quantify the level of trace metals or organic compounds"-- Provided by publisher "This book covers all aspects of environmental trace analysis from sampling through to preparation of the sample to the analytical techniques used to quantify the level of trace metals or organic compounds. The book is divided into two areas: sample preparation for inorganic analysis and sample preparation for organic analysis. This allows the reader to focus on key aspects related to the preparation of samples for their subsequent analysis. Selected case studies provide the reader with the opportunity to consider how the sample preparation approach can be optimized for their own area of expertise"-- Provided by publisher Bibliography Includes bibliographical references and index Notes Print version record and CIP data provided by publisher Subject Environmental chemistry -- Methodology. Sampling. Trace analysis -- Methodology. Form Electronic book LC no. 2013028463 ISBN 1118682793 (Adobe PDF) 111868284X (ePub) 1118683420 (electronic bk.) 1119962706 (hardback) 1119962714 (paper) 9781118682791 (Adobe PDF) 9781118682845 (ePub) 9781118683422 (electronic bk.) 9781119962700 (hardback) 9781119962717 (paper) (hardback)

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