Extraction Methods for Environmental Analysis

302 Pages·1998·3.437 MB·English

by  John R. Dean

Page iii
Extraction Methods for Environmental Analysis
JOHN R. DEAN
University of Northumbria at Newcastle, UK
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Copyright © 1998 John Wiley & Sons Ltd,

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Library of Congress Cataloging-in-Publication Data
Dean. John R.
Extraction methods for environmental analysis / John R. Dean
p. cm.
Includes bibliographical references and index.
ISBN (0-471-98287-3 (cloth : alk. paper)
1. Extraction (Chemistry) 2. Environmental chemistry—Technique.
1. Title
QD63.E88D43 1998 97—48744
628.5'01'543—dc21 CIP
British Library Cataloguing in Publication Data
A catalogue record for this book is available from the British Library
ISBN 0 471 98287 3
Typeset in 10/12 Times by Techset Composition Ltd, Salisbury, England Printed and bound in Great
Britain by Bookcraft (Bath) Ltd This book is printed on acid-free paper responsibly manufactured from
sustainable forestry, in which at least two trees are planted for each one used for paper production
Page v
To
Lynne, Samuel and Naomi
Page vii
CONTENTS
Preface xi
1 1
Environmental Analysis
1. 1 Introduction 1
1.2 Sampling Strategies 3
1.2.1 Sampling Water Matrices 4
1.2.2 Sampling Soils and Sludges 4
1.3 Storage of Samples 5
1.4 Brief Introduction to Practical Chromatographic Analysis 6
1.5 Quality Assurance in Environmental Analysis 10
References 11
Bibliography 11

Part I: Aqueous Samples
2 15
Aqueous Sample Preparation
2.1 Environmental Case Study: Pesticides 15
2.1.1 Environmental Fate and Behaviour of Pesticides 18
References 21
3 23
Classical Approaches for the Extraction of Analytes from Aqueous
Samples
3.1 Liquid-Liquid Extraction 23
3.1.1 Theory of Liquid-Liquid Extraction 23
3.1.2 Solvent Extraction 25
3.1.3 Solvent Evaporation Methods 27
3.2 Purge and Trap for Volatile Organics 33
References 34
4 35
Solid Phase Extraction
4.1 Types of SPE Media 35
4.2 Cartridge or Disk Format 36
4.3 Method of SPE Operation 40
4.4 Solvent Selection 42
Page viii
4.5 Factors Affecting SPE 43
4.6 Selected Methods of Analysis for SPE 43
4.7 Automated and On-line SPE 46
4.8 Selected Applications of Automated On-line SPE 48
References 61
5 63
Solid Phase Microextraction
5.1 Theoretical Considerations 65
5.2 Experimental 66
5.3 Methods of Analysis: SPME-GC 67
5.3.1 Volatile Organics in Water: Direct Extraction 67
5.3.2 Volatile Organics in Water: Headspace Concentration 70
5.3.3 Pesticides from Aqueous Samples 72
5.3.4 Phenols 75
5.3.5 Analysis of Analytes from Solid Matrices 78
5.4 Methods of Analysis: SPME-HPLC 83
5.5 Miscellaneous Applications 84
5.5.1 Characterisation of Alcoholic Beverages 84
5.5.2 Analysis of Human Breath 86
5.5.3 Analysis of Cigarette Smoke Condensate 88
5.5.4 Headspace SPME of Cinnamon 88
5.5.5 Tetraethylead and Inorganic Lead in Water 90
5.5.6 Solid Phase Microextraction-Electrodeposition Device 90
5.5.7 Analysis of Polar Analytes using Derivatisation/SPME 90
References 94
Bibliography 94

Part II: Solid Samples
6 99
Solid Sample Preparation
6.1 Introduction 101
References 106
7 107
Liquid-Solid Extraction
7.1 Introduction 107
7.2 Experimental 107
7.3 Selected Methods of Analysis 109
7.3.1 Soxhlet 110
7.3.2 Soxtec (Automated Soxhlet) 110
7.3.3 Shake-Flask 112
7.3.4 Shake-Flask versus Sonication 114
7.3.5 Shake-Flask versus Reflux (Soxhlet) 117
7.3.6 Sonication versus Soxhlet 118
7.3.7 Other Approaches 119
References 121
123
8
Supercritical Fluid Extraction
8.1 Definition of a Supercritical Fluid 125