Manual of pesticide residue analysis, volume 2

DFG Manual of Pesticide Residue Analysis Volume II VCH © VCH Verlagsgesellschaft mbH, D-6940 Weinheim (Federal Republic of Germany), 1992 Distribution: VCH, P.O Box 101161, D-6940 Weinheim (Federal Republic of Germany) Switzerland: VCH, P.O Box, CH-4020 Basel (Switzerland) United Kingdom and Ireland: VCH (UK) Ltd., Wellington Court, Cambridge CB1 1HZ (England) USA and Canada: VCH, 220 East 23rd Street, New York NY 10010-4606 (USA) ISBN 3-527-27017-5 (VCH, Weinheim) ISBN 0-89573-957-7 (VCH, New York) DFG Deutsche Forschungsgemeinschaft Manual of Pesticide Residue Analysis Volume II Edited by Hans-Peter Thier and Jochen Kirchhoff Working Group "Analysis" Pesticides Commission VCH Deutsche Forschungsgemeinschaft Kennedyallee 40 D-5300 Bonn Telefon: (0228) 885-1 Telefax: (0228) 8852221 Published jointly by VCH Verlagsgesellschaft mbH, Weinheim (Federal Republic of Germany) VCH Publishers Inc., New York, NY (USA) Translators: J Edwards t and Carole Ann Traedgold Library of Congress Card No applied for A catalogue record for this book is available from the British Library Deutsche Bibliothek Cataloguing-in-Publication Data: Manual of pesticide residue analysis / DFG, Deutsche Forschungsgemeinschaft, Pesticides Commission Ed by Hans-Peter Thier and Jochen Kirchhoff [Transl.: J Edwards and Carole Ann Traedgold] Weinheim; Basel (Swizerland); Cambridge; New York, NY: VCH NE: Thier, Hans-Peter [Hrsg.]; Deutsche Forschungsgemeinschaft / Kommission fur Pflanzenschutz-, Pflanzenbehandlungs- und Vorratsschutzmittel Vol (1992) ISBN 3-527-27017-5 (Weinheim ) ISBN 0-89573 957-7 (New York) © VCH Verlagsgesellschaft mbH, D-6940 Weinheim (Federal Republic of Germany), 1992 Printed on acid-free and chlorine-free paper All rights reserved (including those of translation into other languages) No part of this book may be reproduced in any form - by photoprinting, microfilm, or any other means - nor transmitted or translated into a machine language without written permission from the publishers Registered names, trademarks, etc used in this book, even when not specifically marked as such, are not to be considered unprotected by law Composition: Filmsatz Unger & Sommer GmbH, D-6940 Weinheim Printing: betz-druck Gmbh, D-6100 Darmstadt 12 Printed in the Federal Republic of Germany Preface During more than two decades, the Working Group on Pesticide Residue Analysis of the "Senatskommission fur Pflanzenschutz-, Pflanzenbehandlungs- und Vorratsschutzmittel" (Pesticides Commission), Deutsche Forschungsgemeinschaft (DFG), has edited a loose-leaf Manual of residue analytical methods All the methods contained in this Manual were validated prior to their publication, by at least one independent laboratory Therefore, the Manual has met with acceptance far beyond the frontiers of the Federal Republic of Germany, particularly since many of the methods are included in the List of Recommended Methods of Analysis issued by the Codex Committee on Pesticide Residues (CCPR) of the FAO/WHO Codex Alimentarius Commission Many residue analysts are, however, not well versed in German Therefore, to overcome this language barrier and to render the methods accessible to a far wider international circle of analysts, the Working Group decided to translate the most important sections of the Manual into English This mission was sponsored by the Deutsche Forschungsgemeinschaft Volume of the English edition was published in 1987 It contained 23 compound-specific ("single") analytical methods selected from the 6th and 7th instalments (issued in 1982 and 1984, respectively) of the German edition, 17 multiresidue analytical methods and cleanup methods (both 1984 status) as well as all pertinent general sections, e g on the collection and preparation of samples, on the limits of detection and determination, and on micro methods and equipment for sample processing The present Volume of the English edition is a direct continuation and completion of the first volume It contains 32 single methods, many of them designed for the determination of recently developed compounds These methods were adopted, in most cases, from the 8th to 11th instalments of the German edition issued between 1985 and 1991 Furthermore, Volume contains five new multiresidue analytical methods (coded S) published in German since the first volume went to press, and some tables providing supplementary data on the broad applicability of Methods S and S 19 and Cleanup Method 6, both described in Volume Special features of Volume are Part 5, presenting six multiple methods for analysis of residues in water (coded W), and Part on analytical methods for determining residues in water using the Automated Multiple Development (AMD) technique Moreover, two new cleanup methods for the solid-phase extraction of water samples on alkyl-modified silica gel are included An additional chapter introduces a new concept for deriving the limits of detection and determination by the calibration curve technique, thus providing a commendable alternative to the procedure proposed in Volume Finally, a comprehensive table gives massspectrometric El data for confirmation of gas-chromatographic results In some cases, the Editorial Committee has also partly changed or updated the original German version in order to better adjust it to the needs of today's methodology A cumulative index for Volumes and provides easy access to all pertinent compounds and information The Working Group on Pesticide Residue Analysis had hoped that it would render a major contribution to pesticide residue analytical methodology by carrying on the German and English editions However, the Working Group had to terminate its activities in 1989, after so many years of engagement in matters of pesticide residue analysis, because the Senate of VI Preface the DFG modified the basic structures of its advisory commissions with the consequence that the mandate of the Pesticides Commission and its Working Groups expired Nevertheless, the Editorial Committee (J Kirchhoff (chairman), H Frehse, H.-G Nolting, H.-P Thier) was charged, by the DFG, with the commitment to finalize any going publication activities Thus, the Committee first edited the last, 11th Instalment (issued 1991) of the German Manual on the basis of the validated methods that had become available yet by 1989 Next, the Editorial Committee did its very best to compile Volume of the English edition Parts of it are based on the very competent contributions of the late James Edwards (died 1987) who had translated the text of Volume The remaining text was basically translated by Carole Ann Traedgold and edited by the Committee The Editorial Committee hopes that this two-volume compilation of procedures and methods will prove useful to all concerned with the analysis of pesticide residues Contents Contents of Volume Senate Commission for Pesticides, Deutsche Forschungsgemeinschaft Working Group on Residue Analysis, Senate Commission for Pesticides Part 1: Introduction and Instructions (contd.) Derivation of the Limits of Detection and Determination Applying the Calibration Curve Concept Mass-Spectrometric El Data for Confirmation of Results Part 2: Cleanup Methods (contd.) Cleanup Method Cleanup of crude extracts from plant and animal material by gel permeation chromatography on a polystyrene gel in an automated apparatus (updated) Cleanup Method Solid phase extraction of water samples on alkyl-modified silica gel using disposable columns Cleanup Method Solid phase extraction of water samples on alkyl-modified silica gel Part 3: Individual Pesticide Residue Analytical Methods (contd.) Amitrole, 4-A*) Anilazine, 186 Benomyl, Carbendazim, Thiophanate-methyl, 261-378-370 Bitertanol, 613-A Bitertanol, Triadimefon, Triadimenol, 613-425-605 Bromoxynil, Ioxynil, 264-212 Carbendazim, 378 Carbosulfan, Carbofuran, 658-344 Chlorflurenol, Flurenol, 275-215 Chloridazon, 89-A Chlorsulfuron, Metsulfuron, 664-672 Copper Oxychloride, 147-A Cymoxanil, 513 2,4-D, Dichlorprop, 27-A-38-A Dichlobenil, 225-A Dichlofluanid, Tolylfluanid, 203-371 Dichlofluanid, Tolylfluanid, 203-A-371-A Dinobuton, Binapacryl, 255-8 Fonofos, 288 Fosetyl, 522 IX XI XV 25 31 37 41 49 59 69 77 87 99 107 113 127 135 145 153 157 163 169 177 191 197 205 211 *) Code numbers according to which the analytical methods are identified in the German issue of the Manual The number without affixed letter corresponds to the BBA registration number of the individual compound VIII Contents Glufosinate, 651 Glyphosate, 405 Metaldehyde, 151-A Metribuzin, 337 Nitrothal-isopropyl, 416 Oxamyl, 441 Phenmedipham, 233-B Propachlor, 310 Propiconazole, 624 Sulphur, 184-B Thiabendazole, 256-A Thiabendazole, 256-B 217 229 239 245 253 261 269 275 281 287 291 295 Part 4: Multiple Pesticide Residue Analytical Methods (contd.) Pesticides, Chemically Related Compounds and Metabolites Determinable by the Multiresidue Methods in Parts to 6: Supplement to the Table of Compounds, pp 221 ff, Vol S Organohalogen, Organophosphorus and Triazine Compounds (updated) S 19 Organochlorine, Organophosphorus, Nitrogen-Containing and Other Pesticides (updated) S 22 Natural Pyrethrins, Piperonyl Butoxide S 23 Pyrethroids S 24 Organotin Compounds S 25 Methyl Carbamate Insecticides S 26 Phthalimides 317 323 333 343 349 359 Part 5: Multiple Pesticide Residue Analytical Methods for Water W Phenoxyalkanoic Acid Herbicides W Fungicides W Organochlorine Insecticides W Phenoxyalkanoic Acid Herbicides W Triazine Herbicides W 13 Desalkyl Metabolites of Chlorotriazine Herbicides 369 377 387 393 403 413 Part 6: Pesticide Residue Analytical Methods for Water Using the AMD Technique Thin-Layer Chromatographic Analysis of Pesticides and Metabolites Using the Automated Multiple Development (AMD) Technique Examples for Applying the AMD Technique to the Determination of Pesticide Residues in Ground and Drinking Waters Cumulative Indexes for Volumes and Index of Determinable Pesticides, Metabolites and Related Compounds (Index of Compounds) Index of Analytical Materials List of Suppliers Referenced in the Text-Matter of the Manual Author Index 301 313 423 435 449 459 479 483 Contents of Volume Senate Commission for Pesticides, Deutsche Forschungsgemeinschaft Members and Guests of the Working Group on Residue Analysis, Senate Commission for Pesticides Part 1: Introduction and Instructions Explanations Notes on Types and Uses of Methods Important Notes on the Use of Reagents Abbreviations Preparation of Samples Collection and Preparation of Soil Samples Collection and Preparation of Water Samples Use of the Term "Water" Micro Methods and Equipment for Sample Processing Limits of Detection and Determination Reporting of Analytical Results Use of Forms in the Reporting of Analytical Results Part 2: Cleanup Methods Cleanup Method Separation of organochlorine insecticides from hexachlorobenzene and polychlorinated biphenyls Cleanup Method Cleanup of crude extracts from plant and animal material by sweep codistillation Cleanup Method Cleanup of crude extracts from plant material by gel permeation chromatography on Sephadex LH-20 Cleanup Method Cleanup of crude extracts from plant material by gel permeation chromatography on polystyrene gels Cleanup Method Cleanup of large quantities of fats for analysis of residues of organochlorine and organophosphorus compounds Cleanup Method Cleanup of crude extracts from plant and animal material by gel permeation chromatography on a polystyrene gel in an automated apparatus Part 3: Individual Pesticide Residue Analytical Methods Acephate, Methamidophos, 358-365 Aldicarb, 250 Captafol, 266 Captafol, 266-A Captan, 12-A Chlorthiophos, 465 Dalapon, 28 Dichlobenil, 225 X Contents of Volume Diclofop-methyl, 424 Ethylene Thiourea, 389 Folpet, 91-A Heptenophos, 427 Metalaxyl, 517 Methomyl, 299 1-Naphthylacetic Acid, 434 Nitrofen, 340 Paraquat, 134-A Pirimicarb, 309 Pirimiphos-methyl, 476 Pyrazophos, 328 Tetrachlorvinphos, 317 Triazophos, 401 Vinclozolin, 412 Part 4: Multiple Pesticide Residue Analytical Methods Pesticides, Chemically Related Compounds and Metabolites Determinable by the Multiresidue Methods (Table of Compounds) S6 Substituted Phenyl Urea Herbicides S 6-A Substituted Phenyl Urea Herbicides S Triazine Herbicides S Organohalogen, Organophosphorus and Triazine Compounds S9 Organochlorine and Organophosphorus Pesticides S 10 Organochlorine and Organophosphorus Pesticides S 11 Potato Sprout Suppressants Propham and Chlorpropham S 12 Organochlorine Pesticides S 13 Organophosphorus Insecticides S 14 Triazine Herbicides and Desalkyl Metabolites S 15 Dithiocarbamate and Thiuram Disulphide Fungicides S 16 Organophosphorus Pesticides with Thioether Groups S 17 Organophosphorus Insecticides S 18 Bromine-Containing Fumigants S 19 Organochlorine, Organophosphorus, Nitrogen-Containing and Other Pesticides S 20 Phthalimide Fungicides (Captafol, Captan, Folpet) S 21 Ethylene and Propylene Bisdithiocarbamate Fungicides Indexes Index of Determinable Pesticides, Metabolites and Related Compounds (Index of Compounds) Index of Analytical Materials List of Suppliers Referenced in the Text-Matter of the Manual Author Index Index of Analytical Materials Hop foliage Sulphur 2: 287 Instant foods based on milk Organochlorine pesticides 1: 297 Organophosphorus pesticides 1: 297 Jams Bitertanol 2: 77 Vinclozolin 1: 213 Juices* Bitertanol 2: 77, 87 Chlorthiophos 1: 109 Ethylene thiourea 1: 135 Metalaxyl 1: 153 Nitrogen-containing pesticides 1: 383; 2: 317 Organochlorine pesticides 1: 383; 2: 317 Organophosphorus pesticides 1: 383; 2: 317 Tolylfluanid 2: 191 Triadimefon 2: 87 Triadimenol 2: 87 Vinclozolin 1: 213 Kidneys Chlorthiophos 1: 109 Glufosinate 2: 217 Kiwi fruit Glufosinate 2: 217 Kohlrabi Fonofos 2: 205 Heptenophos 1: 149 Methyl carbamate insecticides 2: 349 Nitrogen-containing pesticides 1: 383; 2: 317 Organochlorine pesticides 1: 283, 327, 383; 2: 313, 317 Organophosphorus pesticides 1: 283, 335, 371, 383; 2: 313, 317 Triazine herbicides 1: 283; 2: 313 Lard Organochlorine pesticides 1: 297, 309 Organophosphorus pesticides 1: 297, 309 Leeks Dithiocarbamate fungicides 1: 353 Ethylene thiourea 1: 135 Methyl carbamate insecticides 2: 349 Nitrofen 1: 173 Organochlorine pesticides 1: 283; 2: 313 Organophosphorus pesticides 1: 283, 361; 2: 313 Phenyl urea herbicides 1: 241 467 Leeks (contd.) Pirimiphos-methyl 1: 191 Propachlor 2: 275 Thiuram disulphide fungicides 1: 353 Triazine herbicides 1: 265, 283; 2: 313 Lemons Glufosinate 2: 217 Organochlorine pesticides 1: 327 Triazine herbicides 1: 265 Triazophos 1: 209 Lettuce Acephate 1: 81 Benomyl 2: 69 Bromine-containing fumigants 1: 377 Carbendazim 2: 69 Carbofuran 2: 113 Carbosulfan 2: 113 Chlorthiophos 1: 109 Dichlofluanid 2: 177 Dithiocarbamate fungicides 1: 353, 407 Ethylene thiourea 1: 135 Folpet 1: 143 Fosetyl 2: 211 Heptenophos 1: 149 Metalaxyl 1: 153 Metaldehyde 2: 239 Methamidophos 1: 81 Methomyl 1: 161 Methyl carbamate insecticides 2: 349 Nitrogen-containing pesticides 1: 383; 2: 317 Organochlorine pesticides 1: 283, 383; 2: 313, 317 Organophosphorus pesticides 1: 283, 335, 361, 371, 383; 2: 313, 317 Oxamyl 2: 261 Phenyl urea herbicides 1: 241 Phthalimide fungicides 1: 401 Phthalimides 2: 359 Piperonyl butoxide 2: 323 Pirimicarb 1: 183 Pirimiphos-methyl 1: 191 Pyrethrins 2: 323 Thiophanate-methyl 2: 69 Thiuram disulphide fungicides 1: 353 Tolylfluanid 2: 177 Triazine herbicides 1: 265, 283; 2: 313 Liver Chlorthiophos 1: 109 Glufosinate 2: 217 468 Index of Analytical Materials Maize cobs Metalaxyl 1: 153 Tetrachlorvinphos 1: 203 Maize, green matter Chlorthiophos 1: 109 Metalaxyl 1: 153 Triazophos 1: 209 Maize, kernels Acephate 1: 81 Carbofuran 2: 113 Carbosulfan 2: 113 Chlorthiophos 1: 109 Fonofos 2: 205 Glufosinate 2: 217 Heptenophos 1: 149 Methamidophos 1: 81 Phenyl urea herbicides 1: 241 Propachlor 2: 275 Pyrethroids 2: 333 Triazine herbicides 1: 265 Triazophos 1: 209 Maize, leaves Metalaxyl 1: 153 Phenyl urea herbicides 1: 241 Triazine herbicides 1: 265 Maize, stalks Metalaxyl 1: 153 Phenyl urea herbicides 1: 241 Triazine herbicides 1: 265 Mandarine oranges Chlorthiophos 1: 109 Organochlorine pesticides 1: 283, 327; 2: 313 Organophosphorus pesticides 1: 283; 2: 313 Triazine herbicides 1: 283; 2: 313 Mangold Chloridazon 2: 135 Diclofop-methyl 1: 127 Phenmedipham 2: 269 Piperonyl butoxide 2: 323 Pyrethrins 2: 323 Margarine Organochlorine pesticides 1: 297, 309 Organophosphorus pesticides 1: 297, 309 Meat Chlorthiophos 1: 109 Glufosinate 2: 217 Nitrogen-containing pesticides 1: 383; 2: 317 Organochlorine pesticides 1: 297, 309, 383; 2: 317 Organophosphorus pesticides 1: 297, 309, 383; 2: 317 Meat products* Glufosinate 2: 217 Nitrogen-containing pesticides 1: 383; 2: 317 Organochlorine pesticides 1:297, 309, 383; 2: 317 Organophosphorus pesticides 1: 297, 309, 383; 2: 317 Melons Bitertanol 2: 87 Nitrogen-containing pesticides 1: 383; 2: 317 Organochlorine pesticides 1: 327, 383; 2: 317 Organophosphorus pesticides 1: 383; 2: 317 Organotin compounds 2: 343 Pyrazophos 1: 197 Triadimefon 2: 87 Triadimenol 2: 87 Milk, condensed see Condensed milk Milk, fresh, milk powder Nitrogen-containing pesticides 1: 383; 2: 317 Organochlorine pesticides 1:297, 309,383; 2: 317 Organophosphorus pesticides 1: 297, 309, 383; 2: 317 Milled cereal products Bromine-containing fumigants Mirabellas Glufosinate 1: 377 2: 217 Mud (sludge) Diclofop-methyl 1: 127 Mushrooms Bromine-containing fumigants 1: 377 Dalapon 1: 117 Organochlorine pesticides 1: 283; 2: 313 Organophosphorus pesticides 1: 283; 2: 313 Pirimiphos-methyl 1: 191 Triazine herbicides 1: 283; 2: 313 Mushrooms, dried Bromine-containing fumigants 1: 377 Index of Analytical Materials Must Amitrole 2: 49 Cymoxanil 2: 157 Dichlofluanid 2: 177, 191 Nitrogen-containing pesticides 1: 383; 2: 317 Organochlorine pesticides 1: 383; 2: 317 Organophosphorus pesticides 1: 383; 2: 317 Tolylfluanid 2: 177 Triadimefon 2: 87 Triadimenol 2: 87 Nectarines Organotin compounds 2: 343 Nuts Bromine-containing fumigants 1: 377 Nitrogen-containing pesticides 1: 383; 2: 317 Organochlorine pesticides 1: 383; 2: 317 Organophosphorus pesticides 1: 383; 2: 317 Oat, grains Bromine-containing fumigants 1: 377 Heptenophos 1: 149 Nitrogen-containing pesticides 1: 383; 2: 317 Organochlorine pesticides 1: 383; 2: 317 Organophosphorus pesticides 1: 383; 2: 317 Phenyl urea herbicides 1: 241, 251 Triazine herbicides 1: 265 Oat, straw Phenyl urea herbicides 1: 241, 251 Triazine herbicides 1: 265 Oil seeds* Bitertanol 2: 87 Carbofuran 2: 113 Carbosulfan 2: 113 Chlorthiophos 1: 109 Diclofop-methyl 1: 127 Glufosinate 2: 217 Glyphosate 2: 229 Metalaxyl 1: 153 Nitrogen-containing pesticides 1: 383; 2: 317 Organochlorine pesticides 1: 383; 2: 317 Organophosphorus pesticides 1: 383; 2: 317 Oxamyl 2: 261 Phenyl urea herbicides 1: 241, 251 Pirimiphos-methyl 1: 191 Pyrethroids 2: 333 Triazine herbicides 1: 265 Triazophos 1: 209 Vinclozolin 1: 213 469 Oils, vegetable* see Fats, vegetable Olive oil Organochlorine pesticides 1: 297, 309 Organophosphorus pesticides 1: 297, 309 Pirimiphos-methyl 1: 191 Onions, bulbs Anilazine 2: 59 Bromine-containing fumigants 1: 377 Fonofos 2: 205 Metalaxyl 1: 153 Nitrofen 1: 173 Nitrogen-containing pesticides 1: 383; 2: 317 Organochlorine pesticides 1: 383; 2: 317 Organophosphorus pesticides 1: 361, 383; 2: 317 Phenyl urea herbicides 1: 241 Pirimiphos-methyl 1: 191 Propachlor 2: 275 Pyrethroids 2: 333 Triazine herbicides 1: 265 Vinclozolin 1: 213 Onions, stalks Vinclozolin 1: 213 Orange juice Metalaxyl 1: 153 Orange peel Metalaxyl 1: 153 Thiabendazole 2: 291, 295 Oranges Glufosinate 2: 217 Heptenophos 1: 149 Metalaxyl 1: 153 Organochlorine pesticides 1: 283; 2: 313 Organophosphorus pesticides 1: 283; 2: 313 Oxamyl 2: 261 Pirimiphos-methyl 1: 191 Triazine herbicides 1: 265, 283; 2: 313 Triazophos 1: 209 Parsley Bromine-containing fumigants 1: 377 Organochlorine pesticides 1: 283; 2: 313 Organophosphorus pesticides 1: 283; 2: 313 Triazine herbicides 1: 283; 2: 313 470 Index of Analytical Materials Peaches Bitertanol 2: 87 Captafol 1: 93 Chlorthiophos 1: 109 Dithiocarbamate fungicides 1: 353 1-Naphthylacetic acid 1: 167 Nitrogen-containing pesticides 1: 383; 2: 317 Organochlorine pesticides 1: 283, 383; 2: 313, 317 Organophosphorus pesticides 1: 283, 383; 2: 313, 317 Organotin compounds 2: 343 Oxamyl 2: 261 Pyrazophos 1: 197 Tetrachlorvinphos 1: 203 Thiuram disulphide fungicides 1: 353 Triadimefon 2: 87 Triadimenol 2: 87 Triazine herbicides 1: 265, 283; 2: 313 Vinclozolin 1: 213 Peanut foliage Oxamyl 2: 261 Peanut oil Organochlorine pesticides 1: 297, 309 Organophosphorus pesticides 1: 297, 309 Peanut shells Bitertanol 2: 87 Oxamyl 2: 261 Peanuts Bitertanol 2: 87 Nitrogen-containing pesticides 1: 383; 2: 317 Organochlorine pesticides 1: 383; 2: 317 Organophosphorus pesticides 1: 383; 2: 317 Oxamyl 2: 261 Pirimiphos-methyl 1: 191 Pear juice, pear conserves Tolylfluanid 2: 191 Pears Amitrole 2: 49 Bitertanol 2: 77, 87 Captan 1: 105 Dichlobenil 2: 169 Dithiocarbamate fungicides 1: 353 1-Naphthylacetic acid 1: 167 Nitrogen-containing pesticides 1: 383; 2: 317 Organochlorine pesticides 1: 283, 383; 2: 313, 317 Pears (contd.) Organophosphorus pesticides 1: 283, 335, 383; 2: 313, 317 Phenyl urea herbicides 1: 241 Phthalimide fungicides 1: 401 Pirimiphos-methyl 1: 191 Thiuram disulphide fungicides 1: 353 Tolylfluanid 2: 191 Triadimefon 2: 87 Triadimenol 2: 87 Triazine herbicides 1: 265, 283; 2: 313 Vinclozolin 1: 213 Peas Ethylene thiourea 1: 135 Glufosinate 2: 217 Glyphosate 2: 229 Metalaxyl 1: 153 Phenyl urea herbicides 1: 241 Pirimiphos-methyl 1: 191 Propachlor 2: 275 Triazine herbicides 1: 265 Pepper seeds Metalaxyl 1: 153 Nitrogen-containing pesticides 1: 383; 2: 317 Organochlorine pesticides 1: 383; 2: 317 Organophosphorus pesticides 1: 383; 2: 317 Peppers, sweet Anilazine 2: 59 Heptenophos 1: 149 Nitrogen-containing pesticides 1: 383; 2: 317 Organochlorine pesticides 1: 283, 327, 383; 2: 313, 317 Organophosphorus pesticides 1: 283, 335, 383; 2: 313, 317 Oxamyl 2: 261 Pirimiphos-methyl 1: 191 Triadimefon 2: 87 Triadimenol 2: 87 Triazine herbicides 1: 283; 2: 313 Pineapples Metalaxyl 1: 153 Nitrogen-containing pesticides 1: 383; 2: 317 Organochlorine pesticides 1: 283, 383; 2: 313, 317 Organophosphorus pesticides 1: 283, 335, 383; 2: 313, 317 Triazine herbicides 1: 265, 283; 2: 313 Index of Analytical Materials Plums Acephate 1: 81 Bitertanol 2: 77, 87 Chlorthiophos 1: 109 Glufosinate 2: 217 Methamidophos 1: 81 1-Naphthylacetic acid 1: 167 Nitrogen-containing pesticides 1: 383; 2: 317 Organochlorine pesticides 1: 283, 383; 2: 313, 317 Organophosphorus pesticides 1: 283, 383; 2: 313, 317 Organotin compounds 2: 343 Piperonyl butoxide 2: 323 Pyrethrins 2: 323 Triazine herbicides 1: 265, 283; 2: 313 Vinclozolin 1: 213 Plums: jam, puree Bitertanol 2: 77 Poppy seeds Phenyl urea herbicides Potato peel Thiabendazole 1: 251 2: 291 Potato tops Metribuzin 2: 245 Potatoes Anilazine 2: 59 Captafol 1: 93 Chlorpropham 1: 321 Chlorthiophos 1: 109 Cymoxanil 2: 157 2,4-D 2: 163 Dalapon 1: 117 Dichlorprop 2: 163 Dithiocarbamate fungicides 1: 353, 407 Ethylene thiourea 1: 135 Glufosinate 2: 217 Heptenophos 1: 149 Metalaxyl 1: 153 Metribuzin 2: 245 Nitrogen-containing pesticides 1: 383; 2: 317 Organochlorine pesticides 1: 283, 327, 383; 2: 313, 317 Organophosphorus pesticides 1: 283, 335, 361, 383; 2: 313, 317 Oxamyl 2: 261 Phenyl urea herbicides 1: 241 Phthalimides 2: 359 471 Potatoes (contd.) Piperonyl butoxide 2: 323 Propham 1: 321 Pyrazophos 1: 197 Pyrethrins 2: 323 Pyrethroids 2: 333 Thiuram disulphide fungicides 1: 353 Triazine herbicides 1: 265, 283; 2: 313 Triazophos 1: 209 Vinclozolin 1: 213 Poultry meat Organochlorine pesticides 1: 297, 309 Organophosphorus pesticides 1: 297, 309 Radicchio Anilazine 2: 59 Radishes Fonofos 2: 205 Metaldehyde 2: 239 Methyl carbamate insecticides 2: 349 Organochlorine pesticides 1: 283; 2: 313 Organophosphorus pesticides 1: 283; 2: 313 Propachlor 2: 275 Triazine herbicides 1: 265, 283; 2: 313 Vinclozolin 1: 213 Radishes, small Captafol 1: 93 Dithiocarbamate fungicides 1: 353 Fonofos 2: 205 Heptenophos 1: 149 Organochlorine pesticides 1: 283; 2: 313 Organophosphorus pesticides 1: 283, 335; 2:313 Pirimiphos-methyl 1: 191 Thiuram disulphide fungicides 1: 353 Triazine herbicides 1: 265, 283; 2: 313 Triazophos 1: 209 Vinclozolin 1: 213 Rape, green matter Anilazine 2: 59 Carbofuran 2: 113 Carbosulfan 2: 113 Dithiocarbamate fungicides 1: 353 Glufosinate 2: 217 Pyrethroids 2: 333 Thiuram disulphide fungicides 1: 353 472 Index of Analytical Materials Rape, seeds Carbofuran 2: 113 Carbosulfan 2: 113 Chlorthiophos 1: 109 Diclofop-methyl 1: 127 Glufosinate 2: 217 Glyphosate 2: 229 Pyrethroids 2: 333 Triazophos 1: 209 Vinclozolin 1: 213 Rape, straw Vinclozolin 1: 213 Rape oil Chlorthiophos 1: 109 Rye, grains Bromine-containing fumigants 1: 377 Captafol 1: 99 Nitrogen-containing pesticides 1: 383; 2: 317 Organochlorine pesticides 1: 383; 2: 317 Organophosphorus pesticides 1: 383; 2: 317 Phenyl urea herbicides 1: 241 Propiconazole 2: 281 Triadimefon 2: 87 Triadimenol 2: 87 Triazine herbicides 1: 265 Rye, green matter Captafol 1: 99 Propiconazole 2: 281 Triadimefon 2: 87 Triadimenol 2: 87 Raspberries Dichlofluanid 2: 177 Pirimiphos-methyl 1: 191 Tolylfluanid 2: 177 Triazine herbicides 1: 265 Vinclozolin 1: 213 Rye, straw Captafol 1: 99 Phenyl urea herbicides 1: 241 Propiconazole 2: 281 Triadimefon 2: 87 Triadimenol 2: 87 Triazine herbicides 1: 265 Red beet, edible root Chloridazon 2: 135 Diclofop-methyl 1: 127 Dithiocarbamate fungicides 1: 353 Phenmedipham 2: 269 Thiuram disulphide fungicides 1: 353 Sage Bromine-containing fumigants Red beet, foliage Chloridazon 2: 135 Diclofop-methyl 1: 127 Savoy cabbage Acephate 1: 81 Chlorthiophos 1: 109 Methamidophos 1: 81 Organophosphorus pesticides Red cabbage Fonofos 2: 205 Organochlorine pesticides 1: 283; 2: 313 Organophosphorus pesticides 1: 283, 335, 361, 371; 2: 313 Phenyl urea herbicides 1: 241 Pirimiphos-methyl 1: 191 Triazine herbicides 1: 265, 283; 2: 313 Red currants see Currants, red Rice, grains Pirimiphos-methyl 1: 191 Pyrazophos 1: 197 1: 377 Organochlorine pesticides 1: 297, 309 Organophosphorus pesticides 1: 297, 309 1: 335 Skim milk powder Organochlorine pesticides 1: 297 Organophosphorus pesticides 1: 297 Sludge (mud) Diclofop-methyl 1: 127 Small radishes see Radishes, small Soil Aldicarb 1: 87 Amitrole 2: 49 Anilazine 2: 59 Index of Analytical Materials Soil (contd.) Binapacryl 2: 197 Bitertanol 2: 77, 87 Bromoxynil 2: 99 Captafol 1: 93 Carbendazim 2: 107 Carbofuran 2: 113 Carbosulfan 2: 113 Chlorflurenol 2: 127 Chloridazon 2: 135 Chlorsulfuron 2: 145 Chlorthiophos 1: 109 Cymoxanil 2: 157 Dalapon 1: 117 Dichlobenil 1: 123; 2: 169 Diclofop-methyl 1: 127 Dinobuton 2: 197 Dithiocarbamate fungicides 1: 353 Flurenol 2: 127 Fonofos 2: 205 Glufosinate 2: 217 Glyphosate 2: 229 Heptenophos 1: 149 Ioxynil 2: 99 Metalaxyl 1: 153 Methomyl 1: 161 Metribuzin 2: 245 Metsulfuron 2: 145 Nitrothal-isopropyl 2: 253 Organotin compounds 2: 343 Oxamyl 2: 261 Paraquat 1: 177 Phenyl urea herbicides 1: 241, 251 Phthalimide fungicides 1: 401 Phthalimides 2: 359 Pirimicarb 1: 183 Pirimiphos-methyl 1: 191 Propachlor 2: 275 Propiconazole 2: 281 Pyrazophos 1: 197 Pyrethroids 2: 333 Sulphur 2: 287 Tetrachlorvinphos 1: 203 Thiuram disulphide fungicides 1: 353 Triadimefon 2: 87 Triadimenol 2: 87 Triazine herbicides 1: 265, 347 Triazine herbicides, desalkyl metabolites 1: 347 Triazophos 1: 209 Vinclozolin 1: 213 Sorghum Triazine herbicides 1: 265 473 Sour cherries Glufosinate 2: 217 Vinclozolin 1: 213 Soybean oil Chlorthiophos 1: 109 Organochlorine pesticides 1: 297, 309 Organophosphorus pesticides 1: 297, 309 Soybeans Chlorthiophos 1: 109 Diclofop-methyl 1: 127 Glufosinate 2: 217 Phenyl urea herbicides 1: 241 Triazine herbicides 1: 265 Spelt, grains Phenyl urea herbicides 1: 241 Triazine herbicides 1: 265 Spices (herbs) see Herbs (spices) Spinach Anilazine 2: 59 Chlorthiophos 1: 109 Metalaxyl 1: 153 Metaldehyde 2: 239 Organochlorine pesticides 1: 283; 2: 313 Organophosphorus pesticides 1: 283, 335, 361, 371; 2: 313 Piperonyl butoxide 2: 323 Pyrethrins 2: 323 Triazine herbicides 1: 265, 283; 2: 313 Strawberries Aldicarb 1: 87 Dichlofluanid 2: 177, 191 Dithiocarbamate fungicides 1: 353 Fosetyl 2: 211 Heptenophos 1: 149 Metalaxyl 1: 153 Metaldehyde 2: 239 Methomyl 1: 161 Methyl carbamate insecticides 2: 349 Nitrogen-containing pesticides 1: 383; 2: 317 Organochlorine pesticides 1: 283, 327, 383; 2: 313, 317 Organophosphorus pesticides 1: 283, 335, 383; 2: 313, 317 Organotin compounds 2: 343 Phenmedipham 2: 269 Phenyl urea herbicides 1: 241 474 Index of Analytical Materials Strawberries (contd.) Pirimiphos-methyl 1: 191 Sulphur 2: 287 Tetrachlorvinphos 1: 203 Thiuram disulphide fungicides 1: 353 Tolylfluanid 2: 177, 191 Triazine herbicides 1: 265, 283; 2: 313 Vinclozolin 1: 213 Strawberry plants Aldicarb 1: 87 Suet (tallow) Organochlorine pesticides 1: 297, 309 Organophosphorus pesticides 1: 297, 309 Sugar, raw Vinclozolin 1: 213 Sugar beet, dry chips Vinclozolin 1: 213 Sugar beet, edible root Aldicarb 1: 87 Bitertanol 2: 77, 87 Carbofuran 2: 113 Carbosulfan 2: 113 Chloridazon 2: 135 Chlorthiophos 1: 109 Dithiocarbamate fungicides 1: 353 Glufosinate 2: 217 Glyphosate 2: 229 Heptenophos 1: 149 Metalaxyl 1: 153 Nitrogen-containing pesticides 1: 383; 2: 317 Organochlorine pesticides 1: 383; 2: 317 Organophosphorus pesticides 1: 383; 2: 317 Organotin compounds 2: 343 Phenmedipham 2: 269 Piperonyl butoxide 2: 323 Propachlor 2: 275 Pyrethrins 2: 323 Pyrethroids 2: 333 Thiuram disulphide fungicides 1: 353 Triadimefon 2: 87 Triadimenol 2: 87 Triazine herbicides 1: 265 Vinclozolin 1: 213 Sugar beet, foliage Bitertanol 2: 77, 87 Chloridazon 2: 135 Chlorthiophos 1: 109 Sugar beet, foliage (contd.) Dithiocarbamate fungicides 1: 353 Glufosinate 2: 217 Glyphosate 2: 229 Metalaxyl 1: 153 Organotin compounds 2: 343 Phenmedipham 2: 269 Thiuram disulphide fungicides 1: 353 Triadimefon 2: 87 Triadimenol 2: 87 Sugar beet, syrup Vinclozolin 1: 213 Sugar cane Triazine herbicides 1: 265 Sunflower oil Glufosinate 2: 217 Organochlorine pesticides 1: 297, 309 Organophosphorus pesticides 1: 297, 309 Phenyl urea herbicides 1: 241 Sunflower seeds Glufosinate 2: 217 Metalaxyl 1: 153 Phenyl urea herbicides 1: 241 Triazine herbicides 1: 265 Sweet corn Triazophos 1: 209 Sweet peppers see Peppers, sweet Tallow (suet) see Suet (tallow) Tea, tealike products Bitertanol 2: 77 Nitrogen-containing pesticides 1: 383; 2: 317 Organochlorine pesticides 1: 383; 2: 317 Organophosphorus pesticides 1: 383; 2: 317 Tobacco Ethylene thiourea 1: 135 Metalaxyl 1: 153 Nitrogen-containing pesticides 1: 383; 2: 317 Organochlorine pesticides 1: 383; 2: 317 Organophosphorus pesticides 1: 383; 2: 317 Oxamyl 2: 261 Phenyl urea herbicides 1: 241 Pyrazophos 1: 197 Index of Analytical Materials Tomato juice Ethylene thiourea 1: 135 Tomato leaves Metribuzin 2: 245 Vinclozolin 1: 213 Tomatoes Acephate 1: 81 Anilazine 2: 59 Bitertanol 2: 77 Carbofuran 2: 113 Carbosulfan 2: 113 Chlorthiophos 1: 109 Cymoxanil 2: 157 Dichlofluanid 2: 177 Dithiocarbamate fungicides 1: 407 Ethylene thiourea 1: 135 Folpet 1: 143 Heptenophos 1: 149 Metalaxyl 1: 153 Methamidophos 1: 81 Methomyl 1: 161 Methyl carbamate insecticides 2: 349 Metribuzin 2: 245 Nitrogen-containing pesticides 1: 383; 2: 317 Organochlorine pesticides 1: 283, 327, 383; 2: 313, 317 Organophosphorus pesticides 1: 283, 335, 361, 383; 2: 313, 317 Organotin compounds 2: 343 Oxamyl 2: 261 Phenyl urea herbicides 1: 241 Phthalimide fungicides 1: 401 Piperonyl butoxide 2: 323 Pirimiphos-methyl 1: 191 Pyrethrins 2: 323 Pyrethroids 2: 333 Tolylfluanid 2: 177 Triadimefon 2: 87 Triadimenol 2: 87 Triazine herbicides 1: 283; 2: 313 Triazophos 1: 209 Vinclozolin 1: 213 Turnips, foliage and edible root Anilazine 2: 59 Vegetable fats and oils* Chlorthiophos 1: 109 Glufosinate 2: 217 Nitrogen-containing pesticides 1: 383; 2: 317 Organochlorine pesticides 1: 297, 309, 383; 2: 317 475 Vegetable fats and oils* (contd.) Organophosphorus pesticides 1: 297, 309, 383; 2:317 Phenyl urea herbicides 1: 241 Pirimiphos-methyl 1: 191 Vegetables, dried and fresh Bromine-containing fumigants 1: 377 Water Acephate 1: 81 Amitrole 2: 49, 442 Anilazine 2: 59 Azinphos-ethyl 2: 435 Azinphos-methyl 2: 435 Benalaxyl 2: 437 Bendiocarb 2: 437 Bentazone 2: 437 Binapacryl 2: 197 Bitertanol 2: 77, 87, 435 Bromacil 2: 435 Bromoxynil 2: 99 Captafol 1: 93 Carbofuran 2: 435 Chlorflurenol 2: 127 Chloridazon 2: 135 Chlorotriazine desalkyl metabolites 2: 413 Chlorsulfuron 2: 145 Chlorthiophos 1: 109 Cymoxanil 2: 157, 435 Dalapon 1: 117 Desalkyl metabolites of chlorotriazines 2:413 Dichlobenil 1: 123; 2: 169 Dinobuton 2: 197 Dinoseb 2: 437 Dinoterb 2: 437 Diuron 2: 435 DNOC 2: 437 Ethylene thiourea 1: 135 Fluazifop-P-butyl 2: 437 Flurenol 2: 127 Fluroxypyr-(l-methylheptyl) 2: 437 Fonofos 2: 205 Fosetyl 2: 211 Fungicides 2: 377 Glufosinate 2: 217 Glyphosate 2: 229 Haloxyfop-(2-ethoxyethyl) 2: 437 Ioxynil 2: 99 Lenacil 2: 435 Metalaxyl 1: 153; 2: 437 Metamitron 2: 435 476 Index of Analytical Materials Water (contd.) Methabenzthiazuron 2: 435 Methamidophos 1: 81 Methomyl 1: 161 Metribuzin 2: 245, 435 Metsulfuron 2: 145 Nitrofen 1: 173 Nitrothal-isopropyl 2: 253, 437 Organochlorine insecticides 2: 387 Organotin compounds 2: 343 Oxamyl 2: 261 Paraquat 1: 177 Parathion 2: 435 Pendimethalin 2: 437 Phenoxyalkanoic acid herbicides 2: 369, 393 Phthalimides 2: 359 Pirimicarb 1: 183 Pirimiphos-methyl 1: 191 Propachlor 2: 275 Propiconazole 2: 281 Pyrethroids 2: 333 Terbumeton 2: 437 Tetrachlorvinphos 1: 203 Triadimefon 2: 87, 435 Triadimenol 2: 87, 435 Triazine herbicides 2: 403 Triazine herbicides, desalkyl metabolites 2: 413 Triclopyr-(2-butoxyethyl) 2: 437 Wheat grains Anilazine 2: 59 Benomyl 2: 69 Bromine-containing fumigants 1: 377 Bromoxynil 2: 99 Captafol 1: 93 Carbendazim 2: 69 Chlorflurenol 2: 127 Dalapon 1: 117 Diclofop-methyl 1: 127 Dithiocarbamate fungicides 1: 353 Ethylene thiourea 1: 135 Flurenol 2: 127 Glufosinate 2: 217 Heptenophos 1: 149 Ioxynil 2: 99 Metribuzin 2: 245 Nitrofen 1: 173 Nitrogen-containing pesticides 1: 383; 2: 317 Organochlorine pesticides 1: 383; 2: 317 Organophosphorus pesticides 1: 383; 2: 317 Phenyl urea herbicides 1: 241, 251 Phthalimides 2: 359 Pirimiphos-methyl 1: 191 Propiconazole 2: 281 Wheat grains (contd.) Pyrazophos 1: 197 Pyrethroids 2: 333 Thiophanate-methyl 2: 69 Thiuram disulphide fungicides Triadimefon 2: 87 Triadimenol 2: 87 Triazine herbicides 1: 265 Triazophos 1: 209 1: 353 Wheat, green matter Anilazine 2: 59 Bromoxynil 2: 99 Dalapon 1: 117 Dithiocarbamate fungicides 1: 353 Ioxynil 2: 99 Phthalimides 2: 359 Propiconazole 2: 281 Thiuram disulphide fungicides 1: 353 Triadimefon 2: 87 Triadimenol 2: 87 Wheat, straw Anilazine 2: 59 Benomyl 2: 69 Captafol 1: 93 Carbendazim 2: 69 Chlorflurenol 2: 127 Dalapon 1: 117 Diclofop-methyl 1: 127 Dithiocarbamate fungicides 1: 353 Ethylene thiourea 1: 135 Flurenol 2: 127 Metribuzin 2: 245 Nitrofen 1: 173 Phenyl urea herbicides 1: 241, 251 Propiconazole 2: 281 Pyrazophos 1: 197 Thiophanate-methyl 2: 69 Thiuram disulphide fungicides 1: 353 Triadimefon 2: 87 Triadimenol 2: 87 Triazine herbicides 1: 265 Whole egg, dried see Dried whole egg Whole milk powder Organochlorine pesticides 1: 297, 309 Organophosphorus pesticides 1: 297, 309 Wine Amitrole 2: 49 Dichlofluanid 2: 177, 191 Index of Analytical Materials Wine (contd.) Ethylene thiourea 1: 135 Folpet 1: 143 Fosetyl 2: 211 Metalaxyl 1: 153 Nitrogen-containing pesticides 1: 383; 2: 317 Organochlorine pesticides 1:383; 2:317 Organophosphorus pesticides 1: 383; 2: 317 Propiconazole 2: 281 Tolylfluanid 2: 177 Triadimefon 2: 87 Triadimenol 2: 87 Vinclozolin 1: 213 * see also special entries 477 Witloof chicory Organochlorine pesticides 1: 283; 2: 313 Organophosphorus pesticides 1: 283; 2: 313 Phenmedipham 2: 269 Triazine herbicides 1: 283; 2: 313 Vinclozolin 1: 213 Youngberries Metalaxyl 1: 153 List of Suppliers Referenced in the Text-Matter of the Manual Aldrich Chemical Co., 1001 West Saint Paul Ave., Milwaukee, WI 53233, USA; Aldrich Europe, Poststr 56, Postfach 2004, D-4054 Nettetal 2, FRG Alltech Associates, Inc., 2051 Waukegan Road, Deerfield, IL 60015, USA; Alltech Europe, Begoniastraat 5, B-9731 Eke, Belgium Alpine AG, Maschinenfabrik, Peter-D6rfler-Str 13-25, D-8900 Augsburg, FRG Analytical Bio-Chemistry Laboratories, 7200 ABC Lane, P.O Box 1097, Columbia, MO 65205, USA; in Europe: N Foss Electric GmbH, Waidmannstr 12b, D-2000 Hamburg 50, FRG Analytichem International, Inc., 24201 Frampton Ave., Harbor City, CA 90710, USA J T Baker Inc., 222 Red School Lane, Phillipsburg, NJ 08865, USA; in Europe: J T Baker B.V., Rijsterborgherweg 20, P.O Box 1, NL-7400 AA Deventer, The Netherlands Becker: see Packard Beckman Instruments Inc., 2500 Harbor Blvd., Fullerton, CA 92634, USA Bender und Hobein GmbH, Lindwurmstr 71-73, Postfach 150229, D-8000 Miinchen 15, FRG J C Binzer Papierfabrik, Berleburger Str 71, D-3559 Hatzfeld 1, FRG Bio-Rad Laboratories, Chemical Division, 3300 Regatta Blvd., Richmond, CA 94804, USA; Heidemannstr 164, Postfach 450133, D-8000 Miinchen 45, FRG Bischoff Analysentechnik und -gerate GmbH, Boblinger Str 23, D-7250 Leonberg, FRG Boehringer Ingelheim KG, D-6507 Ingelheim, FRG Brownlee Labs, 2045 Martin Ave., Santa Clara, CA 95050, USA Camag, Sonnenmattstr 11, CH-4132 Muttenz, Switzerland; Bismarckstr 27-29, D-1000 Berlin 41, FRG; Camag Scientific Inc., P.O Box 563, Wrightsville Beach, NC 28480, USA Carlo Erba Strumentazione S.P.A., Strada Rivoltana, 1-20090 Rodano (Milano), Italy Chemie-Mineralien KG, Loningstr 35, D-2800 Bremen, FRG Chemie und Filter GmbH Verfahrenstechnik, Im Schumachergewann 7, D-6900 Heidelberg, FRG Chromatronix Inc., 2300 Leghorn St., Mt View, CA 94043, USA Chrompack International B.V., Kuipersweg 6, P.O Box 8033, NL-4330 EA Middelburg, The Netherlands; Chrompack Inc., 1130 Route 202, Raritan, NJ 08869, USA Corning Glass Works, Inc., Science Products Division, Corning, NY 14831, USA; Corning Laboratory Products, Prince's Street, Richmond, Surrey TW9 1DZ, U.K Degussa AG, GB/AC GKA, Postfach 110533, D-6000 Frankfurt 11, FRG Desaga GmbH, Postfach 101969, D-6900 Heidelberg 1, FRG Dohrmann Div., Xertex Corp., 3240 Scott Blvd., Santa Clara, CA 95042, USA Dow Corning Corp., P.O Box 994, Midland, MI 48686, USA Du Pont Co., Inc., 1007 Market St., Wilmington, DE 19898, USA; Du Pont de Nemours (Deutschland), Du Pont-Str 1, D-6380 Bad Homburg, FRG EGA-Chemie: see Aldrich Gunther Ehle, Glasinstrumentenfabrik, Holzheimer Str 56 a, D-6250 Limburg, FRG F & M Scientific: see Hewlett-Packard 480 List of Suppliers Finnigan MAT, 355 River Oaks Pkwy., San Jose, CA 95134, USA; Paradise, Hemel Hempstead, Herts HP2 4TG, U.K Fluka A C , CH-9470 Buchs, Switzerland; Fluka Chem Corp., 980 South Second St., Ronkonkoma, NY 11779, USA Gerstel GmbH, Aktienstr 232-234, D-4330 Mulheim/Ruhr 1, FRG Heraeus-Christ: see Heraeus Sepatech Heraeus Quarzschmelze GmbH, Quarzstrafie, D-6450 Hanau, FRG Heraeus Sepatech GmbH, Postfach 1220, D-3360 Osterode, FRG Heraeus-Wittmann GmbH, Englerstr 11, D-6900 Heidelberg 1, FRG Hewlett-Packard Co., Mail Stop 2083, 3000 Hanover St., Palo Alto, CA 94304, USA Hormuth-Vetter: Vetter KG, Malscher Strafle, D-6837 St Leon-Rot 2, FRG ICN Biomedicals, Inc., Chromatography Division, 3300 Hyland Ave., Costa Mesa, CA 92626, USA; Miihlgrabenstr 10, D-5309 Meckenheim, FRG J & W Scientific, 91 Blue Ravine Rd., Folsom, CA, 95630, USA Janke & Kunkel GmbH & Co., KG, Neumagenstr 27, D-7813 Staufen, FRG Janssen Pharmaceutica N.V., B-2340 Beerse, Belgium Johns-Manville: Manville, Ken-Caryl Ranch, P.O Box 5108, Denver, CO 80217, USA Dr H Knauer, Wissenschaftl Gerate KG, Heuchelheimer Str 9, D-6380 Bad Homburg, FRG Kontes Glass Co., Spruce St., P.O Box 729, Vineland, NJ 08360, USA Kontron Instruments, Inc., Plymouth St., Everett, MA 02149, USA Kratos Analytical, Inc., 535 E Crescent Ave., Ramsey, NJ 07446, USA Lehmann & Voss & Co., Alsterufer 19, D-2000 Hamburg 36, FRG LKB Products, Pharmacia LKB, Box 305, S-16126 Bromma, Sweden Macherey-Nagel, Postfach 101352, D-5160 Diiren, FRG Mallinckrodt, Inc., 675 McDonnell Blvd., P.O Box 5840, St Louis, MO 63134, USA Mega: see Carlo Erba Melpar: see Tracor E Merck, Frankfurter Str 250, Postfach 4119, D-6100 Darmstadt, FRG Messer Griesheim GmbH, Industriegase, Homberger Str 12, D-4000 Dtisseldorf, FRG Metrawatt GmbH, Thomas-Mann-Str 16-20, Postfach 1333, D-8500 Niirnberg, FRG Micro Tek Instrument: see Tracor Millipore Corporation, 80 Ashby Rd., Bedford, MA 01730, USA Nopco Chemical Co., 350 Mt Kemble Ave., Morristown, NJ 07960, USA Orlita GmbH & Co KG, Dosiertechnik, Max-Eyth-Str 10, D-6300 GieJkn, FRG Packard Instrument Co., Inc., 2200 Warrenville Rd., Downers Grove, IL 60515, USA Perkin-Elmer Ltd., Maxwell Rd., Beaconsfield, Bucks HP9 1QA, U.K.; The Perkin-Elmer Corp., 761 Main Ave., Norwalk, CT 06859, USA Pharmacia LKB Biotechnology, Bjorkgatan 30, S-75182 Uppsala, Sweden; 800 Centennial Ave., Piscataway, NJ 08854, USA Phase Separations, Deeside Industrial Estate, Queensferry, Clwyd CH5 2LR, U.K.; 140 Water St., Norwalk CT 06854, USA Philips, Scientific and Analytical Equipment Div., Lelyweg 1, NL^7602 EA Almelo, The Netherlands; Philips Scientific, Analytical Div., York St., Cambridge CB1 2PX, U.K Pierce Chemical Co., 3747 N Meridian Rd., P.O Box 117, Rockford, IL 61105, USA; Pierce Europe B.V., P.O Box 1512, NI^3260 BA Oud-Beijerland, The Netherlands List of Suppliers 481 Promochem GmbH, Postfach 1246, D-4230 Wesel, FRG Pye Unicam Ltd., York St., Cambridge CB1 2PX, U.K Quickfit: see Corning W Reiss & Co., Krahenweg 5, D-2000 Hamburg 61, FRG Restek Corp., 110 Benner Circle, Bellefonte, PA 16823, USA Retsch GmbH & Co KG, Rheinische Str 36, Postfach 1554, D-5657 Haan 1, FRG Rheodyne, Inc., P.O Box 996, Cotati, CA 94931, USA Riedel-de Haen AG, Wunstorfer Str 40, Postfach 100262, D-3016 Seelze, FRG Carl Roth GmbH & Co., Schoemperlenstr 1-5, Postfach 211162, D-7500 Karlsruhe 21, FRG Sartorius GmbH, Weender Landstr 94-108, Postfach 3243, D-3400 Gottingen, FRG; Sartorius Corp., 140 Wilbur PL, Bohemia NY 11716, USA Schleicher & Schull, Postfach 4, D-3354 Dassel, FRG; 10 Optical Ave., Keene, NH 03431, USA Schoeffel Instrument Corp., 24 Booker St., Westwood, NJ 07675, USA Schott & Gen., Jenaer Glaswerke, Hattenbergstr 10, Postfach 2480, D-6500 Mainz, FRG; Schott America, Odell Plaza, Yonkers, NY 10701, USA Serva Feinbiochemica GmbH & Co., Carl-Benz-Str 7, Postfach 105260, D-6900 Heidelberg 1, FRG; Serva Biochemicals, 50 A & S Dr., Paramus, NJ 07652, USA Shimadzu Scientific Instruments, Inc., 7102 Riverwood Dr., Columbia MD 21046, USA; Shimadzu Europa, Albert-Hahn-Str 6-10, D-4100 Duisburg 29, FRG Spark Holland B.V., P.O Box 388, NI^7800 AJ Emmen, The Netherlands Spectra-Physics, Autolab Div., 3333 North First St., San Jose, CA 95134, USA Supelco, Inc., Supelco Park, Bellefonte, PA 16823, USA Tracor Instruments, Inc., 6500 Tracor Lane, Austin, TX 78725, USA Valco Instruments Co., Inc., P.O Box 55603, Houston, TX 77255, USA; Valco Europe, Untertannberg 7, CH-6214 Schenkon, Switzerland Varian Instrument Group, 220 Humboldt C t , Sunnyvale, CA 94089, USA Waters Chromatography, 34 Maple St., Milford, MA 01757, USA Weisser: supplied by Hans Otto, Feldstr 26-28, D-2000 Hamburg 6, FRG Whatman Inc., Bridewell PL, Clifton, NJ 07014, USA; Whatman Ltd., Springfield Mill, Maidstone, Kent ME14 2LE, U.K Woelm: see ICN Biomedicals CarlZeiss, Postfach 1369-1380, D-7082 Oberkochen, FRG; One Zeiss Dr., Thornwood, NY 10541, USA Author Index Becker, G 1: 283; 2: 313 Bertrand, A 2: 211 Beutel, P 1: 213; 2: 253 Blacha-Puller, M 1: 183; 2: 99, 145, 197, 211, 275, 359 Bos, U 1: 37 Brauckhoff, S 2: 349 Brennecke, R 2: 59, 77, 87, 177, 377 Bullock, D J W 1: 183, 191 Burger, K 2: 41, 423, 435, 442 Btittler, B 1: 99, 105, 143, 401; 2: 281 Cowell, J E 2: 229 Dick, J P 1: 183 Drescher, N 1: 21, 135; 2: 369 Ebing, W 1: 57, 61, 87, 335, 371, 407 Eichler, D 1: 109; 2: 127, 157, 205, 239, 393 Eichner, M 1: 57, 327, 335 Elzner, J 2: 287 Formica, G 2: 69, 403, 413 Frehse, H 1: 37; 2: Gaudernack, E 1: 65 Giannone, C 2: 69, 403, 413 Gorbach, S 1: 29, 37, 65, 127, 149; 2: Gottschild, D 2: 37 Habersaat, B 1: 51 Hahn, H 1: 321 Hamann, R 2: 169 Hershberger, L W 2: 145 Herzel, F 1: 123, 177 Heupt, W 2: 127, 157 Hezel, U 2: 291 Hild, J 1: 361 Holt, R F 1: 161; 2: 261 Holtz, K.-H 2: Hormann, W D 1: 99, 105, 143, 153, 265, 401; 2: 69, 281, 403 Ipach, R 2: 153 Jarczyk, H J 2: 49, 245 Karlhuber, B 1: 57, 347 Keller, W 1: 117, 135; 2: 135, 163, 253 Kennedy, S H 1: 183 Kettrup, A 2: 169 Kirchhoff, J 1: 29 Kirkland, J J 1: 161 Kohle, H 2: 37, 113, 145, 333, 359, 437 Koflmann, A 1: 87 KoBmann, K 2: 269 Krohn, H 1: 173 Kunzler, K 1: 127 Meemken, H.-A 1: 51 Mollhoff, E 2: 49, 343 Muller, M A 2: 211 Nolting, H.-G 1: 93, 167, 173, 177, 183, 203; 2: 37, 99, 113, 145, 197, 211, 275, 323, 333, 359, 437 Nord, P.-J 2: 229 Otteneder, H 2: 291, 295 Otto, S 1: 117, 135, 213; 2: 135, 163 Pease, H L 1: 161; 2: 261 Pflugmacher, J 1: 57, 61, 335, 371, 407 Ramsteiner, K 1: 57, 153, 251, 347 Reding, M A 2: 229 Richtarsky, G W 1: 167 Schmidt, G 1: 177 Schmidt, M 2: 169 Schulte, E 1: 51 Siebers, J 1: 81, 183, 191; 2: 99, 113, 145, 197, 211, 275, 323, 333, 359 Slates, R V 2: 145 Sochor, H 2: 217 Specht, W 1: 71, 75, 309, 383; 2: 31, 107, 317 Stijve, T 1: 297, 377 Thier, H.-P 1: 17, 29, 37, 71, 167, 297, 309, 321, 353, 361, 377, 383; 2: 3, 317, 323, 349 Thier, W 1: 197, 209 Vogel, W 2: 239 Vogeler, K 2: 191, 377 Voss, G 1: 241 Walter, H.-F 2: Weil, L : ; 2: 387 Weinmann, W D 1: 21, 37, 81, 93, 167, 173, 177, 183, 191, 203, 2: 323 Winkler, S 1: 65 Wolf, A 1: 93, 203 Zahnow, E W 2: 145 [...]... of measurements The measured values listed in Table 1 will be used for this purpose Table 1 Measured values from recovery experiments Example 1 Concentration [|ig/kg] Added (X) Found (Y) 0 20 40 80 100 120 170 20 0 12 26 45 63 105 115 153 180 Example 2 Concentration [mg/kg] Added (X) Found (Y) 0.03 0.03 0.03 0.03 0.05 0.05 0.05 0.05 0.1 0.1 0.1 0.1 0 .2 0 .2 0 .2 0 .2 0.031 0. 027 0. 029 0. 025 0.037 0.0 42. .. = n — 2 degrees of freedom (in the following text designated as "t" only) sR = y —- E (Yj - A - BXj )2 = standard error of estimate: "mean" deviation of the signal values Y{ from the calibration line Limits of Detection and Determination 15 With £ ( Y - A - B X ) 2 = M - L2/K, the standard error can also be expressed as 6.4 Confidence limits of X = (Y - A ) / B for given signal value Y K 2 C = B2 - (t... 3 can be considered the arithmetic mean of X{ and X 2 with good approximation X 2 is corresponding to LDC* (Figure 4) and X£ v (Figure 5) Xj and X 2 can be calculated from the formulae IIa and l i b (see 6.6, see also 3 .2) Limits of Detection and Determination 3 Limit of detection (LDC) 3.1 Definition The limit of detection is defined by the smallest content of the analyte in an analytical sample,... level, a, the limit of detection for an analyte is derived from the calibration curve It is represented by the smallest value X L D C for which the confidence intervals of the corresponding signal value Y LDC and of the signal value for a "nil" content do not overlap (Figure 2) X=0 LDC X = Concentration Fig 2 Definition of the limit of detection (LDC) 3 .2 Decision rules The limit of detection corresponds,... omitted 9.1 Example 1: Calculation of LDC and LDM Note that in this case only one measurement per fortification level was made Number of measurements: n = 8 Limits of Detection and Determination 19 When proceeding according to 6.1 and 6 .2, the following results will be obtained: E F G H J = 730 = 101700 = 699 = 86873 = 93670 X= 91 .25 , K = L = M= N = 35087.50 29 886 .25 25 797.88 25 456.01 Y = 87.38 The terms... C) and IV, one obtains LDC = 48.83 Eq V yields Y c = 71 .28 Y c is the Y value, on the calibration line, for X = Xl 20 Limits of Detection and Determination 20 40 i 80 100 120 140 160 180 20 0 Cone, added X (ug/kg) LDC=48.830 LDM= 72. 3486 Fig 6 Evaluation of Example 1 by computer Calibration curve with prediction interval; S = 95% Therefore, Xr = 72. 35 (cf eq VI) X c v and Y c v are obtained from eqs VII... the point of intersection, YUP, to the point where it intersects the lower limit of the prediction interval This point corresponds, on the abscissa, to the value of LDC, the limit of detection (cf 9.3) For computer calculation of LDC, see 6.6 4 Limit of determination (LDM) 4.1 Definition Residue analyses are frequently performed to monitor foodstuff for compliance with established maximum residue limits... 1 At the limit of detection, the probability for the false proof of detecting the analyte which in reality is not present in the sample (error of the first kind) is just equivalent to the selected a of 5% This is illustrated in Figure 2: The distribution curves for the signal values A and YLDC each overlap by 2. 5 area percent, corresponding to a test with a = 5% (two-sided) The error of the second kind... K D (ST. )2 = (B V o ) 2 - ^ L J ^- = auxiliary term; K (Vo )2 = 0.04 6. 12 Calculation of Y c v The value for Y, corresponding to the point of intersection, is calculated by inserting Xcv in (VIII): (VIII) Y c v = (A + B • X c v ) • (1 + t • Vo) 6.13 Calculation of X m (IX) X m = (Y c v -A)/B 7 References C / Bailey, E.A Cox and J.A Springer, High pressure liquid chromatographic determination of the intermediates/side... series of measurements, the use of a suitably programmed computer is recommended In individual cases, both limits can be derived graphically, with relatively little calculation effort and with sufficient accuracy, from a plot of the calibration curve and its prediction interval For an example, see 9.3 Limits of Detection and Determination 5 2 Calibration curve concept 2. 1 Basic considerations The aim of