John wiley sons extraction methods for environmental analysisdean 1998 chromatography

Page iii Extraction Methods for Environmental Analysis JOHN R DEAN University of Northumbria at Newcastle, UK Page iv Copyright © 1998 John Wiley & Sons Ltd, Baffins Lane, Chichester, West Sussex PO19 IUD, England National 01243 779777 International ( +44) 1243 779777 e-mail (for orders and customer service enquiries): cs-books@wiley.co.uk Visit our Home Page on http://www.wiley.co.uk or http:// www.wiley.com 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, scanning or otherwise, except under the terms of the Copyright Designs and Patents Act 1988 or under the terms of a licence issued by the Copyright Licensing Agency, 90 Tottenham Court Road London WIP 9HE, UK, without the permission in writing of the Publisher Other Wiley Editorial Offices John Wiley & Sons, Inc., 605 Third Avenue, New York NY 10158-0012, USA WILEY -VCH Verlag GmbH, Pappelallee 3, D-69469 Weinheim, Germany Jacaranda Wiley Ltd 33 Park Road, Milton, Queensland 4064 Australia John Wiley & Sons (Asia) Pte Ltd, Clementi Loop #02-01, Jin Xing Distripark, Singapore 129809 John Wiley & Sons (Canada) Ltd, 22 Worcester Road, Rexdale, Ontario M9W ILI, Canada 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) Extraction (Chemistry) Environmental chemistry—Technique 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 471 98287 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 Environmental Analysis 1 Introduction 1.2 Sampling Strategies 1.2.1 Sampling Water Matrices 1.2.2 Sampling Soils and Sludges 1.3 Storage of Samples 1.4 Brief Introduction to Practical Chromatographic Analysis 1.5 Quality Assurance in Environmental Analysis 10 References 11 Bibliography 11 Part I: Aqueous Samples Aqueous Sample Preparation 2.1 Environmental Case Study: Pesticides 2.1.1 Environmental Fate and Behaviour of Pesticides References Classical Approaches for the Extraction of Analytes from Aqueous Samples 3.1 Liquid-Liquid Extraction 15 15 18 21 23 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 Solid Phase Extraction 35 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 Solid Phase Microextraction 63 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 Solid Sample Preparation 99 6.1 Introduction 101 References 106 Liquid-Solid Extraction 107 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 Supercritical Fluid Extraction 8.1 Definition of a Supercritical Fluid 125 2, 4-dimethylphenol 79, 88, 89, 158, 206 2, 5-dimethylphenol 88, 89 2, 6-dimethylphenol 88, 89 dimethylphthalate 155, 157, 159, 176 di-n-butylphthalate 157, 159 4, 6-dinitro-2-methylphenol 175 2, 4-dinitrophenol 79, 158, 175 dinoseb 51 dinoterb 51 dioctylphthalate 31, 155 dioxabenzofos 204 dioxins 100, 196, 197, 198, 199, 200, 201, 202, 203 diphenyltin 177 Page 223 disulfoton 77 2, 6-di-tert-butyl-4-methylphenol (BHT) 85 diuron 51, 55, 160 E edifenphos 204 endosulfan 3, 73, 77 endosulfan I 75, 76, 157, 185 endosulfan II 76, 77, 149, 157, 185 endosulfan sulphate 73, 75, 76, 77 endrin 3, 75, 76, 77, 78, 149, 157, 174, 185 endrin aldehyde 75, 76, 77, 149 endrin ketone 75, 76, 77, 149 EPN 77, 204 EPTC 77, 78 ethanol 86, 87 ethion 59, 204 ethoprofos 77, 78, 204 ethylbenzene 32, 67, 69, 70, 71, 80 ethyl butyrate 32 ethyl cinnamate 32 2-ethylhexanol 32 ethyl parathion (see parathion-ethyl) 3-ethylphenol 88, 89 4-ethylphenol 88, 89 eugenol 88 F famphur 77 fatty acids 90, 91, 93 fenamiphos 44, 53 fenchlorphos 59 fenchlorovos 77 fenitrothion 3, 53, 59, 77, 204 fenpropidin 19 fenpropimorph 19 fenthion 204 fenuron 55 fluometuron 55, 117, 119 fluoranthene 82, 83, 111, 112, 113, 131, 133, 134, 135, 136, 137, 138, 139, 157, 172, 173, 192, 193, 195 fluorene 83, 85, 111, 112, 136, 137, 138, 157, 159, 172, 173, 193, 195 G geraniol 84, 86 glyphosate 19, 49, 52 H heptachlor 75, 76, 77, 78, 149, 155, 157, 159, 160, 174, 185 heptachlor epoxide 75, 76, 77, 157, 159, 185 2, 3', 4, 4', 5, 6, 6'-heptachlorobiphenyl 157 hexachlorobenzene (HCB) 3, 120, 152, 157, 159, 180, 184, 185 2, 2', 4, 4', 5, 6'-hexachlorobiphenyl 157, 159 hexachlorobutadiene hexachlorocyclopentadiene 159, 184, 185 g-hexachlorohexane hexaconazole 202, 206, 207 hexazinone 54, 77 hydroxyatrazine 54 5-hydroxymethyl-2-formaldehyde (5-HMF) 85 I imazethapyr 175 indeno[1, 2, 3-cd]pyrene 85, 112, 131, 133, 134, 135, 137, 138, 139, 157, 159, 172, 173, 192, 193, 195 iprobenfos 77 isodrin 160 isophorone 31 isopropalin 77 isoprene 86, 87 isoproturon 19, 53, 55, 160 isoxathion 77 K 3-ketocarbofuran L lead 90 lenacil 117, 119 linalool 84, 86 lindane 2, 77, 159, 174 linuron 53, 55, 117, 119 M malathion 3, 202, 204 mancozeb 19 maneb 19 MCPA 19 mecoprop 19 mecoprop-P 19 mercury metamitron 19, 51 metazachlor 51 methabenzthiazuron 53, 55 methamidophos 201, 204 methidathion 204 methiocarb sulfone methiocarb sulfoxide methoxychlor 75, 76, 77, 157, 159, 173 2-methoxyphenol 88, 89 3-methoxyphenol 88, 89 4-methoxyphenol 88, 89 n-methylaniline 80 Page 224 methyl chloropyrifos (see chlorpyrifos methyl) 2-methyl-4, 6-dinitrophenol 79, 158 methyl hexadecanoate 84 methylmercury 178 2-methylnapthalene 31, 111 methylparathion (see parathion-methyl) 2-methylphenol 206 metobromuron 51 metolachlor 77, 78, 148, 150 metoxuron 55 metribuzin 77, 117, 119 metsulfuron methyl 151, 153 mevinphos 59 mirex 155 molinate 77 monobutyltin 177, 178 monolinuron 55 monomethyl metoxuron 51 monophenyltin 177 monuron 55 N naphthalene 2, 32, 80, 111, 112, 132, 136, 137, 138, 157, 172, 173, 193, 195 1-naphthol 88, 89 2-naphthol 88, 89 neburon 55 nerol 84, 86 nerol oxide 84, 86 nitralin 51 nitrofen 51, 114, 116, 117 2-nitrophenol 51, 79, 158 4-nitrophenol 79, 158 nonylphenol ethoxylate 84 O oxadiazon 77 oxyfluorofen 77 2, 2', 3, 3', 4, 5', 6, 6'-octachlorobiphenyl 159 P palmitic acid 92 parathion 53, 59 parathion-ethyl 77 parathion-methyl 77 PCB 26 140, 145 PCB 28 110, 140, 141, 142, 144, 145, 197 PCB 44 145 PCB 52 110, 140, 141, 142, 144, 145, 197 PCB 101 110, 140, 141, 142, 144, 145, 197 PCB 105 110, 141, 142, 144 PCB 118 110, 140, 141, 142, 144, 145 PCB 128 110, 141, 142, 144, 145 PCB 138 110, 140, 141, 142, 144, 197 PCB 149 110, 141, 142, 144 PCB 153 110, 140, 141, 142, 144, 197 PCB 156 110, 141, 142, 144 PCB 163 110 PCB 170 110, 141, 142, 144 PCB 180 110, 140, 141, 142, 144, 145, 197 PCB 209 180 pebulate 77 pendimethalin 19, 77 pentachlorobenzene 180 2, 2', 3', 4, 6-pentachlorobiphenyl 156, 159 pentachlorophenol 3, 57, 79, 111, 139, 141, 146, 147, 157, 158, 159 perchloroethylene 32 perylene 133, 134, 159 phenanthrene 83, 85, 111, 112, 113, 131, 133, 134, 135, 136, 137, 138, 139, 157, 159, 172, 192, 193, 195 phenol 36, 52, 55, 565, 57, 79, 88, 89, 145, 154, 158, 175, 184, 185, 172, 192, 193, 195 phosalone 202, 204 phosphonate 154 phoxim 51 pirimiphos-methyl 204 profluralin 77, 114, 116, 117 prometon(e) 18, 54 prometryn(e) 17, 18, 60 propachlor 77 propanil 53 propazine 17, 18, 51, 54, 59, 60, 72, 77, 78, 160 propionic acid 91 propyzamide 117, 119 prothiofos 77, 204 putrescine 90 pyrazophos 59 pyrene 82, 83, 85, 111, 112, 113, 131, 133, 134, 135, 136, 137, 138, 139, 157, 159, 172, 173, 192, 193, 195 Q quinoline 31 S sebuthylazine 54 secbumeton 59 simazine 3, 17, 18, 53, 54, 59, 60, 72, 78, 117, 118, 119, 157, 159, 160 simetryn(e) 18, 54 Page 225 stearic acid 92 sulfamethazine 154 sulfotep 59, 77 sulfur 19 sulfuric acid 18, 19 T TDE 152 O,O,O-TEP 77 terbacil 77 terbuthylazine 54, 59 terbutryn(e) 17, 18 α-terpineol 84, 86 1, 2, 3, 5-tetrachlorobenzene 180 1, 2, 4, 5-tetrachlorobenzene 180 2, 2', 4, 4'-tetrachlorobiphenyl 157, 159 2, 3, 4, 5-tetrachlorophenol 141, 146 2, 3, 4, 6-tetrachlorophenol 141, 146, 147 2, 3, 5, 6-tetrachlorophenol 141, 146, 147 tetrachlorvinphos 59 tetraethyllead 90 thionazin 77 toluene 32, 63, 67, 69, 70, 71 tolunitrile 32 toxaphene 159 trans-nonachlor 159 tri-allate 19, 114, 116, 117 triazophos 59 tributyltin 3, 177, 178 trichlorobenzene 1, 2, 3-trichlorobenzene 180 1, 2, 4-trichlorobenzene 180 1, 3, 5-trichlorobenzene 180 2, 4, 5-trichlorobiphenyl 157, 159 trichloroethene 82 trichloroethylene 32 2, 3, 5-trichlorophenol 141, 146 2, 3, 6-trichlorophenol 147 2, 4, 5-trichlorophenol 147 2, 4, 6-trichlorophenol 57, 79, 147, 158 tridemorph 19 trietazine 17, 59, 72, 160 triethyl citrate 85 trifluralin 3, 19, 51, 60, 77, 78 2, 4, 6-trimethylphenol 88, 89 triphenylene 136, 139 triphenyltin 3, 177 triprolidine 154 triton X-100 84 V vanillin 88, 89 valeric acid 91 vernolate 77 W warfarin 51 X xylene 2, 63, 67, 82 m-xylene 69, 70, 71, 80 o-xylene 69, 70, 71, 80 p-xylene 69, 70, 71, 80 ...Page iii Extraction Methods for Environmental Analysis JOHN R DEAN University of Northumbria at Newcastle, UK Page iv Copyright © 1998 John Wiley & Sons Ltd, Baffins Lane, Chichester,... 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) Extraction (Chemistry) Environmental. .. Park Road, Milton, Queensland 4064 Australia John Wiley & Sons (Asia) Pte Ltd, Clementi Loop #02-01, Jin Xing Distripark, Singapore 129809 John Wiley & Sons (Canada) Ltd, 22 Worcester Road, Rexdale,