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Environmental Trace Analysis: Techniques and Applications

ISBN: 978-1-119-96270-0
278 pages
December 2013
Environmental Trace Analysis: Techniques and Applications (1119962706) cover image

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.

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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

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Professor John Dean, Professor of Analytical and Environmental Science, Northumbria University, UK
Fellow of the Royal Society of Chemistry (FRSC); Chartered Chemist (C.Chem.); Chartered Scientist (C.Sci.); Registered Analytical Chemist
John 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.

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  • 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
  • Divided into two areas: sample preparation for inorganic analysis and sample preparation for organic analysis
  • 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
See More

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