Environmental Trace Analysis - John R. Dean - E-Book

Environmental Trace Analysis E-Book

John R. Dean

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Beschreibung

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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Veröffentlichungsjahr: 2013

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Contents

Cover

Title Page

Copyright

Dedication

About the Author

Preface

Acknowledgements

Acronyms and Abbreviations

Chapter 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

Chapter 2: Investigative Approach for Environmental Analysis

2.1 Introduction

2.2 Recording of Practical Results

2.3 Significant Figures

2.4 Units

2.5 Summary

Appendix

Further Reading

Chapter 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

3.7 Summary

References

Further Reading

Chapter 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

Chapter 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

Chapter 6: Preparation of Environmental Solid Samples for Inorganic Analysis

6.1 Introduction

6.2 Decomposition Techniques

6.3 Selective Extraction Methods

6.4 Physiologically-Based Extraction Test or in vitro Gastrointestinal Extraction

6.5 Earthworms

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

Chapter 7: Preparation of Environmental Liquid Samples for Inorganic Analysis

7.1 Introduction

7.2 Liquid–Liquid Extraction of Metals

7.3 Ion Exchange

7.4 Co-Precipitation

7.5 Summary

References

Further Reading

Chapter 8: Preparation of Environmental Solid Samples for Organic Analysis

8.1 Introduction

8.2 Liquid–Solid Extraction

8.3 Pressurised Fluid Extraction

8.4 Microwave-Assisted Extraction

8.5 Supercritical Fluid Extraction

8.6 Matrix Solid Phase Dispersion

8.7 Physiologically-Based Extraction Test or In Vitro Gastrointestinal 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)

References

Further Reading

Chapter 9: Preparation of Environmental Liquid Samples for Organic Analysis

9.1 Introduction

9.2 Liquid–Liquid Extraction

9.3 Solid Phase Extraction

9.4 Purge and Trap Extraction

9.5 Headspace Extraction

9.6 Solid Phase Microextraction

9.7 Stir-Bar Sorptive Extraction

9.8 Microextraction in a Packed Syringe

9.9 Liquid Phase Microextraction

9.10 Membrane Extraction

9.11 A Comparison of Extraction Techniques

9.12 Summary

References

Further Reading

Chapter 10: Preparation of Environmental Air Samples for Organic Analysis

10.1 Introduction

10.2 Thermal Desorption

10.3 Summary

Further Reading

Chapter 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

11.4 Summary

Further Reading

Chapter 12: Instrumental Techniques for Environmental Trace Analysis

12.1 Introduction

12.2 Environmental Inorganic Analysis

12.3 Environmental Organic Analysis

12.4 Other Techniques for Environmental Organic Analysis

12.5 Portable Techniques for Field Measurements

12.6 Summary

Further Reading

Chapter 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

13.11 Summary

References

Chapter 14: Some Numerical Worked Examples

14.1 Introduction

Index

This edition first published 2014

© 2014 John Wiley & Sons, Ltd

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The advice and strategies contained herein may not be suitable for every situation. In view of ongoing research, equipment modifications, changes in governmental regulations, and the constant flow of information relating to the use of experimental reagents, equipment, and devices, the reader is urged to review and evaluate the information provided in the package insert or instructions for each chemical, piece of equipment, reagent, or device for, among other things, any changes in the instructions or indication of usage and for added warnings and precautions. The fact that an organization or Website is referred to in this work as a citation and/or a potential source of further information does not mean that the author or the publisher endorses the information the organization or Website may provide or recommendations it may make. Further, readers should be aware that Internet Websites listed in this work may have changed or disappeared between when this work was written and when it is read. No warranty may be created or extended by any promotional statements for this work. Neither the publisher nor the author shall be liable for any damages arising herefrom.

Library of Congress Cataloging-in-Publication Data

Dean, John R., author.

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

pages cm

Includes bibliographical references and index.

ISBN 978-1-119-96270-0 (hardback) — ISBN 978-1-119-96271-7 (pbk.)

1. Trace analysis—Methodology. 2. Environmental chemistry—Methodology. 3. Sampling. I. Title.

TD193.D428 2014

577.27028′7–dc23

2013024965

A catalogue record for this book is available from the British Library.

HB ISBN: 978-1-119-96270-0

PB ISBN: 978-1-119-96271-7

To my wife LynneAnd our children Sam and Naomi

About the Author

John R. Dean D.Sc., Ph.D., D.I.C., M.Sc., B.Sc., FRSC, C.Chem., CSci. Cert.Ed.

John R. Dean took his first degree in Chemistry at the University of Manchester Institute of Science and Technology (UMIST), followed by an M.Sc. in Analytical Chemistry and Instrumentation at Loughborough University of Technology and finally a Ph.D. and D.I.C. in Physical Chemistry at Imperial College of Science and Technology, London. He then spent two years as a postdoctoral research fellow at the Food Science Laboratory of the Ministry of Agriculture, Fisheries and Food in Norwich in conjunction with Polytechnic South West in Plymouth. This was followed by a temporary lectureship in Inorganic Chemistry at Huddersfield Polytechnic. In 1988 he was appointed to a lectureship in Inorganic/Analytical Chemistry at Newcastle Polytechnic (now Northumbria University). This was followed by promotion to Senior Lecturer (1990), Reader (1994), Principal Lecturer (1998) and Associate Dean (Research) (2004). In 2004 he was appointed as Professor of Analytical and Environmental Science. Since 2008 he has held dual responsibility as Head of the Graduate School and Research Professor in the Department of Applied Sciences.

In 1998 he was awarded a D.Sc. (London) in Analytical and Environmental Science and was the recipient of the 23rd SAC Silver Medal in 1995. He has published extensively in analytical and environmental science. He is an active member of the Royal Society of Chemistry Analytical Division (RSC/AD) having served as a member of the atomic spectroscopy group for 15 years (10 as honorary secretary) as well as a past chairman (1997–99); he has been a member of the North East Region RSC/AD since 1992 serving as chairman (2001–03; 2013-present) and Honorary Secretary (2011 onwards). He has served on Analytical Division Council for four terms as well as being Vice-President (2002–04).

He is an active member of Tyne Valley Canoe Club and can be found most weekends on a river, lake or the sea. He has achieved BCU personal performance awards in white water kayaking (4 star leader), sea kayaking (4 star) and open canoe (5 star leader trainee). He holds BCU Level 3 coach status in white water kayaking and sea kayaking and is moderate water endorsed in open canoe. In addition, he is a UKCC Level 3 coach in white water kayaking and a UKCC Level 3 open canoe trainee.

Preface

The field of environmental trace analysis continues to develop and expand both in terms of its application and in the range of analytical techniques that are applied. While this book is not a direct update of a previous publication by the author (Methods for Environmental Trace Analysis, John R. Dean, AnTS, Wiley, 2003: ISBN 0-470-84421-3) it does build upon the knowledge presented. By taking a different style and format to the original text, by updating where appropriate and by adding new areas of investigation that have developed over the intervening 10 years a new text has emerged.

The book is arranged into 14 chapters covering the essentials of good laboratory housekeeping, making and recording practical results, principles of quantitative analysis, through to sampling protocols and sample storage. The book is sub-divided to allow the specific techniques that are used to prepare solid, liquid and, where appropriate, volatile samples for inorganic and organic analyses to be described. Emphasis is also placed on the use of pre-concentration techniques and clean-up procedures for organic samples. Chapter 12 focuses briefly on the wide range of analytical techniques that are applied to environmental trace elemental and organic analyses as well as a consideration of portable techniques for field measurements. Chapter 13 looks at some selected case studies used to highlight the application of the techniques in environmental trace analysis.

Finally, a special mention to all the students (past and present) who have helped to contribute to my interest in the field of environmental trace analysis. Our achievements have been many and varied across a broad area of environmental trace analysis – and mostly enjoyable!

John R. DeanApril 2013

Acknowledgements

Thank you to Lynne Dean for drawing Figures 4.2, 4.3, 4.4, 8.4, 12.11, 12.15(b), 12.16 and 13.8.

Thank you to Naomi Dean for drawing Figure 4.5.

Thank you to Dr Pinpong Kongchana for drawing Figures 8.2 and 8.7 as well as Figures in Box 6.1 illustrating conventional and microwave heating.

Thank you to Edwin Ludkin for drawing Figures 12.15a and 12.19.

Thank you to Thermo Fisher Scientific for permission to publish Figure 12.22; to Geotechnical Services for permission to publish Figure 12.23; to Spectral International, Inc. for permission to publish Figure 12.24; to InPhotonics, Inc. for permission to publish Figure 12.25; to RAE Systems for permission to publish Figure 12.26; and, to Smiths Detection for permission to publish Figure 12.27.

Thank you to Dr Jane Entwistle for Figure 13.1.

Thank you to Dr Nwabueze Elom for Figure 13.2.

Thank you to Dr Katherine Stapleton for Figures 13.3, 13.4 and 13.5.

Thank you to Dr Michael Deary for Figures 13.6 and 13.7.

Acronyms and Abbreviations

AAacetic acidAASatomic absorption spectroscopyAESatomic emission spectroscopyAFSatomic fluorescence spectroscopyAPCIatmospheric pressure chemical ionisationAPDCammonium pyrrolidine dithiocarbamateASEaccelerated solvent extractionBCRCommunity Bureau of ReferenceBSAN, O-bistrimethylsilyl-acetamideBSTFAN,O-bis-trimethylsilyl-trifluoroacetamideBTEXbenzene, toluene, ethylbenzene and xylene'sCCDcharged coupled deviceCIchemical ionisationCIDcharged injection deviceCISEDChemometric Identification of Substrates and Element DistributionsCLEAContaminated Land Exposure AssessmentCOSHHControl of Substances Hazardous to HealthCRMcertified reference materialDadalton (atomic mass unit)DADdiode array detectionDCMdichloromethane (also known as methylene chloride)

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