Thư viện tri thức trực tuyến
Kho tài liệu với 50,000+ tài liệu học thuật
© 2023 Siêu thị PDF - Kho tài liệu học thuật hàng đầu Việt Nam
Environmental Trace Analysis: Techniques and Applications
Nội dung xem thử
Mô tả chi tiết
Environmental
Trace Analysis
Environmental
Trace Analysis
TECHNIQUES AND APPLICATIONS
TECHNIQUES AND APPLICATIONS
John R. Dean
Increasing environmental regulations have resulted in the need for new methods of analysis for
environmental samples. A number of techniques have been developed that reduce or eliminate
the need for toxic organic solvents to be used, and 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.
Building upon the knowledge presented in the author’s previous title, Methods for
Environmental Trace Analysis, this book provides new areas of investigation and over 10 years of
developments.
Environmental Trace Analysis: Techniques and Applications covers the essentials of
• good laboratory housekeeping
• making and recording practical results
• principles of quantitative analysis
• sampling protocols and sample storage
• sample preparation for inorganic analysis
• sample preparation for organic analysis
• the wide range of analytical techniques that are applied to environmental trace elemental
and organic analyses.
Including case studies that highlight the application of the techniques, this book is intended to
provide practical information and a comparison of methods applied to environmental samples.
This text is suitable for students studying environmental science as well as related chemistry
and biology study programmes.
Dean Environmental Trace Analysis : TECHNIQUES AND APPLICATIONS
John R. Dean
Department of Applied Sciences, Northumbria University, UK
Also available
as an e-book
ISBN 978-1-119-96271-7
Environmental Trace Analysis
Environmental
Trace Analysis
Techniques and Applications
John R. Dean
Department of Applied Sciences,
Northumbria University, UK
This edition first published 2014
# 2014 John Wiley & Sons, Ltd
Registered office
JJohn Wiley & Sons Ltd, The Atrium, Southern Gate, Chichester, West Sussex, PO19 8SQ, United
Kingdom
For details of our global editorial offices, for customer services and for information about how to
apply for permission to reuse the copyright material in this book please see our website at www
.wiley.com.
The right of the author to be identified as the author of this work has been asserted in accordance
with the Copyright, Designs and Patents Act 1988.
All rights reserved. No part of this publication may be reproduced, stored in a retrieval system, or
transmitted, in any form or by any means, electronic, mechanical, photocopying, recording or
otherwise, except as permitted by the UK Copyright, Designs and Patents Act 1988, without the prior
permission of the publisher.
Wiley also publishes its books in a variety of electronic formats. Some content that appears in print
may not be available in electronic books.
Designations used by companies to distinguish their products are often claimed as trademarks. All
brand names and product names used in this book are trade names, service marks, trademarks or
registered trademarks of their respective owners. The publisher is not associated with any product or
vendor mentioned in this book.
Limit of Liability/Disclaimer of Warranty: While the publisher and author have used their best efforts
in preparing this book, they make no representations or warranties with respect to the accuracy or
completeness of the contents of this book and specifically disclaim any implied warranties of
merchantability or fitness for a particular purpose. It is sold on the understanding that the publisher is
not engaged in rendering professional services and neither the publisher nor the author shall be liable
for damages arising herefrom. If professional advice or other expert assistance is required, the
services of a competent professional should be sought.
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
577.270280
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
Set in 10.5/13pt, Sabon by Thomson Digital, Noida, India.
1 2014
To my wife Lynne
And our children Sam and Naomi
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
viii CONTENTS
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 þ 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
CONTENTS ix
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 Microwave-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 þ 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
x CONTENTS
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
CONTENTS xi
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
xii CONTENTS
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
CONTENTS xiii