Handbook of Environmental Analysis Second Edition Chemical Pollutants in Air, Water, Soil, and Solid Wastes Pradyot Patnaik Boca Raton London New York CRC Press is an imprint of the Taylor & Francis Group, an informa business CRC Press Taylor & Francis Group 6000 Broken Sound Parkway NW, Suite 300 Boca Raton, FL 33487-2742 © 2010 by Taylor and Francis Group, LLC CRC Press is an imprint of Taylor & Francis Group, an Informa business No claim to original U.S Government works Printed in the United States of America on acid-free paper 10 International Standard Book Number: 978-1-4200-6581-7 (Hardback) This book contains information obtained from authentic and highly regarded sources Reasonable efforts have been made to publish reliable data and information, but the author and publisher cannot assume responsibility for the validity of all materials or the consequences of their use The authors and publishers have attempted to trace the copyright holders of all material reproduced in this 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CCC, a separate system of payment has been arranged Trademark Notice: Product or corporate names may be trademarks or registered trademarks, and are used only for identification and explanation without intent to infringe Library of Congress Cataloging-in-Publication Data Patnaik, Pradyot Handbook of environmental analysis : chemical pollutants in air, water, soil, and solid wastes / author, Pradyot Patnaik 2nd ed p cm Includes bibliographical references and index ISBN 978-1-4200-6581-7 (alk paper) Pollutants Analysis I Title TD193.P38 2010 628.5 dc26 Visit the Taylor & Francis Web site at http://www.taylorandfrancis.com and the CRC Press Web site at http://www.crcpress.com 2009044675 To my brother, Dr Pradipta Patnaik, in loving memory Contents List of Tables xxiii Preface xxvii Preface to the First Edition xxix Acknowledgments xxxi Author xxxiii Glossary of Terms: Units, Conversions, and Abbreviations xxxv PART I Analytical Techniques Introduction Precision and Accuracy of Analysis Quality Assurance and Quality Control in Environmental Analysis Precision and Accuracy Control Charts 7 17 Analysis of Organic Pollutants by Gas Chromatography Selection of Column Detectors Calibration Calculations External Standard Calibration Alternative Calculation Internal Standard Method Routine Analysis 21 22 25 26 27 27 29 29 30 Analysis of Organic Pollutants by Gas Chromatography/Mass Spectrometry Terms and Definitions Application of Mass Spectrometry Interpretation of Mass Spectra Number of Carbon Atoms 31 31 32 33 35 v vi Contents “Nitrogen Rule” Index of Hydrogen Deficiency Determination of Molecular Formula Chemical Ionization Limitation of GC/MS Analysis U.S EPA Methods Volatile Organics by Purge and Trap Method Semivolatile Organics Tuning Compound Identification Calibration References 36 36 36 38 39 39 40 41 42 44 45 47 Extraction of Organic Pollutants and Sample Cleanup Sample Extraction Liquid–Liquid Extraction Solid Phase Extraction Soxhlet Extraction Supercritical Fluid Extraction Cleanup Acid–Base Partitioning Alumina Column Cleanup Silica Gel Cleanup Florisil Column Cleanup Gel-Permeation Cleanup Sulfur Cleanup Permanganate–Sulfuric Acid Cleanup 49 49 49 51 51 52 52 53 54 54 55 55 55 56 Titrimetric Analysis Acid–Base Titration Calculation Oxidation–Reduction Titrations Standardization of Oxidants Reducing Agent Oxidation–Reduction Indicators Iodometric Titration Role of Potassium Iodide Reducing Agent Standardization of Na2S2O3 Starch Indicator Argentometric Titration Complexometric Titrations Potentiometric Titration End Point Detection 57 58 61 64 68 69 70 71 74 74 75 76 77 80 82 83 Colorimetric Analysis 85 Contents Analysis of Metals by Atomic Absorption and Emission Spectroscopy Atomic Spectroscopy: An Overview Sample Digestion for Metals Atomic Absorption Spectrometry Chelation–Extraction Method Hydride Generation Method Cold Vapor Method for Mercury Determination Accuracy in Quantitation Standard Addition Atomic Emission Plasma Spectroscopy Inductively Coupled Plasma Mass Spectrometry Ion-Selective Electrodes Analysis Environmental Sample Analysis Standard Calibration Method Standard Addition Method Sample Addition Method vii 89 90 91 92 94 95 95 96 97 98 98 103 104 105 106 108 10 Application of High-Performance Liquid Chromatography in Environmental Analysis 109 11 Ion Chromatography References 115 119 12 Air Analysis Sampling Plan Air Sampling Direct Collection of Air Use of Adsorbent Tubes Air Sampling for Particulates and Inorganic Substances Flow Rate Chemical Analysis Calculation 121 121 122 122 123 124 125 125 126 13 Application of Immunoassay Techniques in Environmental Analysis Extraction Calculation 131 133 133 PART II Specific Classes of Substances and Aggregate Properties 14 Aldehydes and Ketones Derivatization with 2,4-Dinitrophenylhydrazine Chromatographic Columns and Conditions Sample Collection and Holding Time Air Analysis 137 139 141 141 141 viii Contents 15 Alkalinity Calculation 145 145 16 Bromide Phenol Red Colorimetric Method Procedure Reagents Titrimetric Method Determination of Bromide Plus Iodide Procedure Determination of Iodide Calculation 147 147 148 148 148 149 149 150 150 17 Chloride Mercuric Nitrate Titrimetric Method Procedure Reagents Argentometric Titrimetric Method Procedure Reagents Automated Ferricyanide Colorimetric Method Procedure Reagents Gravimetric Determination of Chloride Procedure Calculation 153 153 154 154 155 155 156 156 156 157 157 157 158 18 Cyanate Calculation Procedure 159 159 160 19 Cyanide, Total Silver Nitrate Titrimetric Method Procedure Reagents Colorimetric Method Procedure Preparation of Cyanide Standards and Calibration Curve Reagents Determination of Cyanide in Soil, Sediment, and Solid Waste Cyanides in Aerosol and Gas 161 161 162 162 162 163 165 166 166 167 20 Cyanide Amenable to Chlorination Procedure Alternative Procedure Reagents 169 169 170 171 21 Emerging Pollutants: Nonionic Surfactants—Alkylphenols and Their Ethoxylates Structures 173 174 Contents Sample Extractions and Analysis: General Discussion SPE–LC/MS Method (Liquid Chromatography Tandem Mass Spectrometry (LC-MS/MS)) SPE–GC/MS Method References ix 175 178 179 182 22 Emerging Pollutants: Organophosphate Flame Retardants, Plasticizers, and Lubricants Analysis of Indoor Dust References 183 188 188 23 Emerging Pollutants: Pharmaceuticals and Personal Care Products U.S EPA Method 1694 Summary of the Method Sample Preparation Sample Cleanup LC-MS/MS Analysis Qualitative Determination and Quantification Quality Assurance/Quality Control Sample Collection, Preservation, and Holding Time References 191 191 191 195 201 201 202 203 204 204 24 Emerging Pollutants: Steroids and Hormones Outline of the Procedure Sample Collection, Preservation, and Storage GC Conditions MS Conditions Calibration and Quantitation Quality Control References 207 207 209 210 210 211 215 215 25 Fluorides Colorimetric SPADNS Method Procedure Automated Colorimetric Method 217 217 218 218 26 Haloacetic Acids Alternative Methods References 219 220 222 27 Halogenated Hydrocarbons Solvent Extraction Sample Collection and Preservation Internal Standards/Surrogates and Tuning Compounds Air Analysis 223 225 228 229 229 x Contents 28 Hardness Hardness Determinations Calculation Titration 233 234 234 234 29 Herbicides: Chlorophenoxy Acid Analysis Sample Extraction Hydrolysis Esterification Gas Chromatographic Analysis Air Analysis 235 235 235 236 237 238 240 30 Herbicides: Glyphosate Water Analysis HPLC Method Sampling and Storage Detection Limit Miscellaneous Methods for Analysis of Glyphosate Residues in Water, Soil, Sludge, Fruit, and Vegetable Extracts References 243 243 243 244 244 31 Hydrocarbons Analysis Total Petroleum Hydrocarbons Gasoline Range Organics Diesel Range Organics 247 248 248 249 250 32 Hydrocarbons, Polynuclear Aromatic HPLC Columns and Conditions GC Columns and Conditions MS Conditions Sample Extraction and Cleanup Air Analysis Reference 253 255 255 255 255 257 258 33 Nitrogen (Ammonia) Sample Distillation Reagents Titrimetric Method Reagents Colorimetric Nesslerization Method Procedure Calculation Reagents and Standards Colorimetric Phenate Method Procedure Calculation Reagents and Standards 259 259 260 260 261 262 262 262 263 264 264 264 265 245 246 Appendix K Type/Class 717 Method # Techniques Compounds CAS No trans-1,3-Dichloropropene 10061-02-6 Halogenated hydrocarbon (VOC) 502.2 524.2 601 624 OLMO1 GC-PID GC/MS GC-HSD GC/MS GC/MS Dichlorvos (Vapona) 62-73-7 Pesticide, organophosphorus 507 8270 GC-NPD GC/MS Dicrotophos (Bidrin) 141-66-2 Pesticide, organophosphorus 8270 GC/MS Dieldrin 60-57-1 Chlorinated pesticide 505 508 608 625 8080 8270 OLMO1 GC-ECD GC-ECD GC-ECD GC/MS GC-ECD GC/MS GC-ECD Diethyl phthalate 84-66-2 Phthalate ester 606 625 8060 8270 OLMO1 GC-ECD GC/MS GC-ECD/FID GC/MS GC/MS Diethylstilbestrol 56-53-1 Phenol 8270 GC/MS Diethyl sulfate 64-67-5 Sulfate ester 8270 GC/MS Dilantin 57-41-0 Heterocyclic nitrogen compound 8270 GC/MS Dimethoate (Cygon) 60-51-5 Pesticide, organophosphorus 8270 GC/MS 3,3-Dimethoxybenzidine 119-90-4 Aromatic amine 8270 GC/MS 7,12-Dimethylbenz[a]anthracene 57-97-6 PAH 8270 GC/MS N,N-Dimethyl-4-(phenylazo) benzenamine 60-11-7 8270 GC/MS Dimethyl phthalate 131-11-3 Phthalate ester 525 606 625 8060 8270 OLMO1 GC/MS GC-ECD GC/MS GC-ECD/FID GC/MS GC/MS 2,4-Dimethylphenol 105-67-9 Phenol 604 625 8040 8270 OLMO1 GC-FID/ECD GC/MS GC-FID/ECD GC/MS GC/MS Dinex (2-cyclohexyl-4,6dinitrophenol) 131-89-5 Nitrophenol 8040 8270 GC-FID GC/MS 1,2-Dinitrobenzene 528-29-0 Nitroaromatic 8270 GC/MS 1,3-Dinitrobenzene 99-65-0 Nitroaromatic 8270 GC/MS 718 Appendix K Type/Class Method # Techniques Compounds CAS No 1,4-Dinitrobenzene 100-25-4 Nitroaromatic 8270 GC/MS 2,4-Dinitrophenol 51-28-5 Phenol 604 625 8040 8270 OLMO1 GC-FID/ECD GC/MS GC-ECD/FID GC/MS GC/MS 2,4-Dinitrotoluene 121-14-2 Nitroaromatic 625 8270 OLMO1 GC/MS GC/MS GC/MS 2,6-Dinitrotoluene 606-20-2 Nitroaromatic 625 8270 OLMO1 GC/MS GC/MS GC/MS Dinoseb 88-85-7 Phenol (nitrophenol pesticide) 515.1 8040 8150 8270 GC-ECD GC-FID GC-ECD GC/MS Dioctyl phthalate 117-84-0 Phthalate ester 606 625 8060 8270 OLMO1 GC-ECD GC/MS GC-ECD/FID GC/MS GC/MS Dioxin (2,3,7,8-TCDD) 1746-01-6 Dioxin 613 8280 GC/MS GC/MS Diphenylamine (N-phenylbenzeneamine) 122-39-4 Aromatic amine 8270 GC/MS 1,2-Diphenyl hydrazine 122-66-7 Azobenzene 8270 GC/MS Diquat dibromide (Aquacide, Reglone) 85-00-7 Triazine pesticide 549 HPLC-UV Disulfoton (Disyston) 298-04-4 Pesticide, organophosphorus 507 8140 8270 GC-NPD GC-FPD GC/MS Disulfoton sulfoxide (oxydisulfoton) 2497-07-6 Pesticide, organophosphorus 507 GC-NPD Dowicide (2,3,4,6-tetrachlorophenol) 58-90-2 Phenol 8270 GC/MS Dursban (Chlorpyrifos) 2921-88-2 Pesticide, organophosphorus 508 8140 GC-ECD GC-FPD Endosulfan-I 959-98-8 Pesticide, chlorinated 508 608 625 8080 8270 OLMO1 GC-ECD GC-ECD GC/MS GC-ECD GC/MS GC-ECD Endosulfan-II (β-endosulfan, thiodan-II) 33213-65-9 Pesticide, chlorinated 508 608 625 GC-ECD GC-ECD GC/MS Appendix K Compounds CAS No Type/Class 719 Method # Techniques 8080 8270 OLMO1 GC-ECD GC/MS GC-ECD Endosulfan sulfate 1031-07-8 Pesticide, chlorinated 508 608 625 8080 OLMO1 GC-ECD GC-ECD GC/MS GC-ECD GC-ECD Endrin 72-20-8 Pesticide, chlorinated 505 508 525 608 625 8080 8270 OLMO1 GC-ECD GC-ECD GC/MS GC-ECD GC/MS GC-ECD GC/MS GC-ECD Endrin aldehyde 7421-93-4 Pesticide, chlorinated 508 608 625 8080 8270 OLMO1 GC-ECD GC-ECD GC/MS GC-ECD GC/MS GC-ECD Endrin ketone 53494-70-5 Pesticide, chlorinated 8270 OLMO1 GC/MS GC-ECD Ethion (Nialate) 563-12-2 Pesticide, organophosphorus 8270 GC/MS Ethoprophos (Ethoprop) 13194-48-4 Pesticide, organophosphorus 507 8140 GC-NPD GC-FPD Ethyl carbamate 51-79-6 Carbamate pesticide 8270 GC/MS Ethyl chloride (chloroethane) 75-00-3 VOC (halocarbon) 502.2 524.2 601 624 8260 OLMO1 GC-ELCD GC/MS GC-HSD GC/MS GC/MS GC/MS Ethylbenzene 100-41-4 VOC (aromatic) 502.2 524.2 602 624 8020 8260 OLMO1 GC-PID GC/MS GC-PID GC/MS GC-PID GC/MS GC/MS Ethylene dibromide (1,2-dibromoethane, EDB) 106-93-4 VOC (halogenated hydrocarbon) 502.2 524.2 8011 8260 GC-ELCD GC/MS GC-ECD GC/MS 720 Appendix K Compounds CAS No Ethylene dichloride (1,2-dichloroethane) 107-06-2 VOC (halogenated hydrocarbon) Bis-(2-Ethylhexyl) adipate Bis-(2-Ethylhexyl) phthalate 103-23-1 117-81-7 Adipate ester Phthalate ester Ethyl methanesulfonate Famphur (Famophos) 62-50-0 52-85-7 Fenamiphos (Nemacur) 22224-92-6 Fensulfothion 115-90-2 Fenthion (Baytex) 55-38-9 Sulfonate Pesticide, organophosphorus Pesticide, organophosphorus Pesticide, organophosphorus Pesticide, organophosphorus Fluoranthene 206-44-0 Polynuclear aromatic hydrocarbon Fluorene (9H-fluorene) 86-73-7 Polynuclear aromatic hydrocarbon o-Fluorophenol Glyphosate 367-12-4 1071-83-6 Heptachlor 76-44-8 Type/Class Phenol Pesticide, organophosphorus Pesticide, chlorinated Method # Techniques 502.2 524.2 601 624 8260 OLMO1 525 525 606 625 8060 8270 OLMO1 8270 8270 GC-ELCD GC/MS GC-HSD GC/MS GC/MS GC/MS GC/MS GC/MS GC-ECD GC/MS GC-ECD/FID GC/MS GC/MS GC/MS GC/MS 507 GC-NPD 8140 8270 8140 GC-FPD GC/MS GC-FPD 8270 550.1 610 625 8310 8270 OLMO1 525 550.1 610 625 8310 8270 OLMO1 8270 547 GC/MS HPLC-FL HPLC-FL GC/MS HPLC-FL GC/MS GC/MS GC/MS HPLC-UV HPLC-UV/ GC-FID GC/MS HPLC-UV GC/MS GC/MS GC/MS HPLC-FL 505 508 525 608 625 8080 8270 OLMO1 GC-ECD GC-ECD GC/MS GC-ECD GC/MS GC-ECD GC/MS GC-ECD Appendix K Compounds CAS No Type/Class Heptachlor epoxide 1024-57-3 Pesticide, chlorinated 721 Method # Techniques 505 508 608 625 GC-ECD GC-ECD GC-ECD GC/MS 8080 8270 OLMO1 GC-ECD GC/MS GC/MS 1,2,3,4,6,7,8-Heptachlorodibenzop-dioxin 35822-46-9 Dioxin 8280 GC/MS Hexachlorobutadiene 87-68-3 Halocarbon 502.2 524.2 612 625 8120 8260 8270 OLMO1 GC-PID/ ELCD GC/MS GC-ECD GC/MS GC-ECD GC/MS GC/MS GC/MS Hexachlorocyclopentadiene 77-47-4 Halogenated hydrocarbon 505 525 612 625 8120 8270 OLMO1 GC-ECD GC/MS GC-ECD GC/MS GC-ECD GC/MS GC/MS 1,2,3,6,7,8-Hexachlorodibenzo-pdioxin 57653-85-7 Dioxin 8280 GC/MS 1,2,3,4,7,8-Hexachlorodibenzofuran 70648-26-9 Dibenzofuran 8280 GC/MS Hexachlorobenzene 118-74-1 Halogenated aromatic 505 508 525 612 625 8120 8270 OLMO1 GC-ECD GC-ECD GC/MS GC-ECD GC/MS GC-ECD GC/MS GC/MS Hexachloroethane 67-72-11 Halocarbon 612 625 8120 8270 OLMO1 GC-ECD GC/MS GC-ECD GC/MS GC/MS Hexachlorophene (Nabac) 70-30-4 Phenol 8270 GC/MS Hexachloropropene 1888-71-7 Chlorinated hydrocarbon 8270 GC/MS Hexamethylphosphoramide 680-31-9 Phosphoric amide 8270 GC/MS 2-Hexanone (methyl butyl ketone) 591-78-6 Ketone OLMO1 GC/MS 722 Appendix K Compounds CAS No Type/Class Hydroquinone Indeno (1,2,3-cd)pyrene 123-31-9 193-39-5 Aromatic ketone Polynuclear aromatic hydrocarbon Isophorone 78-59-1 Ketone Isodrin 465-73-6 Isosafrole Kepone (chlordecone) Kerb 120-58-1 143-50-0 23950-58-5 Leptophos (Phosvel) 21609-90-5 Lindane (γ-BHC) 58-89-9 Chlorinated aromatic Benzodioxole Pesticide, chlorinated Pesticide, chlorinated amide Pesticide, organophosphorus Pesticide, chlorinated Malathion (phosphothion) 121-75-5 Maleic anhydride Mesitylene 108-31-6 108-67-8 Mestranol Metaphos (methyl parathion) 72-33-3 298-00-0 Methapyrilene Methiocarb (Mesurol) Methomyl (Lannate) 91-80-5 2032-65-7 16752-77-5 Methoxychlor 72-43-5 Pesticide, organophosphorus Anhydride Aromatic Steroid Pesticide, organophosphorus Pyridinyl amine Pesticide, carbamate Pesticide, thiocarbamate Pesticide, chlorinated Method # Techniques 8270 525 550.1 610 625 8310 8270 OLMO1 609 625 8270 OLMO1 8270 GC/MS GC/MS HPLC-FL HPLC-FL GC/MS HPLC-FL GC/MS GC/MS GC-FID GC/MS GC/MS GC/MS GC/MS 8270 8270 507 8270 8270 GC/MS GC/MS GC-NPD GC/MS GC/MS 505 508 525 608 8080 8270 OLMO1 8270 GC-ECD GC-ECD GC/MS GC-ECD GC-ECD GC/MS GC-ECD GC/MS 8270 502.2 524.2 8260 8270 8140 8270 8270 531.1 531.1 GC/MS GC-PID GC/MS GC/MS GC/MS GC-FPD GC/MS GC/MS HPLC-FL HPLC-FL 505 508 525 608 8080 8270 OLMO1 GC-ECD GC-ECD GC/MS GC-ECD GC-ECD GC/MS GC-ECD Appendix K Type/Class 723 Method # Techniques Compounds CAS No 3-Methylcholanthrene 56-49-5 PAH 8270 GC/MS Methyl bromide (bromomethane) 74-83-9 VOC (halocarbon) 502.2 524.2 601 624 8260 OLMO1 GC-ELCD GC/MS GC-HSD GC/MS GC/MS GC/MS Methyl chloride (chloromethane) 74-87-3 VOC (halocarbon) 502.2 524.2 601 624 GC-ELCD GC/MS GC-HSD GC/MS 8260 OLMO1 GC/MS GC/MS 604 625 8040 8270 OLMO1 GC-PID GC/MS GC-ECD/FID GC/MS GC/MS 2-Methyl-4,6-dinitrophenol 534-52-1 Phenol Methyl ethyl ketone (2-butanone) 78-93-3 Ketone OLMO1 GC/MS Methyl isobutyl ketone (MIBK) 108-10-1 Ketone OLMO1 GC/MS Methyl methanesulfonate 66-27-3 Sulfonate ester 8270 GC/MS 2-Methylnaphthalene 91-57-6 PAH 8270 OLMO1 GC/MS GC/MS N-Methyl-N-nitrosoethanamine 10595-95-6 Nitrosamine 8270 GC/MS Methylene bromide (dibromomethane) 74-95-3 VOC (halocarbon) 502.2 524.2 8260 GC-ELCD GC/MS GC/MS Methylene chloride (dichloromethane) 75-09-2 VOC (halocarbon) 502.2 524.2 601 624 8260 OLMO1 GC-ELCD GC/MS GC-HSD GC/MS GC/MS GC/MS Metolachlor 51218-45-2 Pesticide, chlorinated 507 GC-NPD Metribuzin 21087-64-9 Pesticide, triazine 507 GC-NPD Mevinphos (Phosdrin) 7786-34-7 Pesticide, organophosphorus 507 8140 8270 GC-NPD GC-FPD GC/MS Mexacarbate 315-18-4 Pesticide, carbamate 8270 GC/MS MOCA (4,4´-Methylene-bis [2-chloroaniline]) 101-14-4 Aromatic amine 8270 GC/MS Monocrotophos 6923-22-4 Pesticide, organophosphorus 8270 GC/MS Naled (Dibrom) 300-76-5 Pesticide, organophosphorus 8140 8270 GC-FPD GC/MS 724 Appendix K Type/Class Method # Techniques Compounds CAS No Naphthalene 91-20-3 PAH 502.2 524.2 550.1 610 625 8260 8270 8310 OLMO1 GC-PID GC/MS HPLC-UV HPLC-UV GC/MS GC/MS GC/MS HPLC-UV GC/MS 1,4-Naphthoquinone (1,4-naphthalenedione) 130-15-4 Aromatic ketone 8270 GC/MS 1-Naphthylamine 134-32-7 Aromatic amine 8270 GC/MS 2-Naphthylamine 91-59-8 Aromatic amine 8270 GC/MS Nicotine 54-11-5 Alkaloid 8270 GC/MS 5-Nitroacenaphthene 602-87-9 Nitroaromatic 8270 GC/MS 2-Nitroaniline (2-nitrobenzenamine) 88-74-4 Nitroaromatic 8270 OLMO1 GC/MS GC/MS 3-Nitroaniline 99-09-2 Nitroaromatic (aromatic amine) 8270 OLMO1 GC/MS GC/MS p-Nitroaniline 100-01-6 Aromatic amine (nitroaromatic) 8270 OLMO1 GC/MS GC/MS 5-Nitro-o-anisidine 99-59-2 Aromatic amine 8270 GC/MS Nitrobenzene 98-95-3 Nitroaromatic 609 625 8270 OLMO1 GC-FID GC/MS GC/MS GC/MS 4-Nitrobiphenyl 92-93-3 Nitroaromatic 8270 GC/MS 2-Nitrophenol 88-75-5 Phenol 604 625 8040 8270 OLMO1 GC-FID/ECD GC/MS GC-FID/ECD GC/MS GC/MS 4-Nitrophenol 100-02-7 Phenol 515.1 604 625 8040 8270 OLMO1 GC-ECD GC-FID/ECD GC/MS GC-ECD/FID GC/MS GC/MS 4-Nitroquinoline-1–oxide 56-57-5 Heterocyclic nitrogen compound 8270 GC/MS GC/MS N-Nitrosodiethylamine 55-18-5 Nitrosamine 8270 N-Nitrosodi-n-butylamine 924-16-3 Nitrosamine 8270 GC/MS N-Nitrosodimethylamine (N-methyl-Nnitrosomethanamine) 62-75-9 Nitrosamine 625 8270 GC/MS GC/MS Appendix K Type/Class 725 Method # Techniques Compounds CAS No N-Nitrosodiphenylamine 86-30-6 Nitrosamine 607 625 8270 OLMO1 GC-NPD GC/MS GC/MS GC/MS Nitrofen (TOK) 1836-75-5 Chlorinated nitroaromatic 8270 GC/MS N-Nitrosodi-n-propylamine 621-64-7 Nitrosamine 625 8270 OLMO1 GC/MS GC/MS GC/MS 4-Nitrosomorpholine 59-89-2 Nitrosamine 8270 GC/MS N-Nitrosopiperidine 100-75-4 Heterocyclic nitrogen compound 8270 GC/MS N-Nitrosopyrrolidine 930-55-2 Nitrosamine 8270 GC/MS 5-Nitro-o-toluidine 99-55-8 Aromatic amine (nitroaromatic) 8270 GC/MS cis-Nonachlor 5103-73-1 Pesticide, chlorinated 505 GC-ECD trans-Nonachlor 39765-80-5 Pesticide, chlorinated 505 525 GC-ECD GC/MS Octachlorodibenzo-p-dioxin (OCDD) 3268-87-9 Dioxin 8280 GC/MS Octamethylpyrophosphoramide 152-16-9 Pesticide, organophosphorus 8270 GC/MS 4,4´-Oxydianiline (4,4´-diaminodiphenyl ether) 101-80-4 Aromatic amine 8270 GC/MS Paraquat 1910-42-5 Pesticide, bipyridinum 549 HPLC-UV Parathion (Niran) 56-38-2 Pesticide, organophosphorus 8270 GC/MS 1,2,3,7,8,-Pentachlorodibenzo-pdioxin 40321-76-4 Dioxin 8280 GC/MS 1,2,3,7,8-Pentachlorodibenzofuran 57117-41-6 Dibenzofuran 8280 GC/MS Pentachlorobenzene 608-93-5 Pesticide, chlorinated 8270 GC/MS Pentachloronitrobenzene 82-68-8 Chlorinated nitroaromatic 8270 GC/MS Pentachlorophenol 87-86-5 Phenol 515.1 525 604 625 8040 8270 OLMO1 GC-ECD GC/MS GC-ECD/FID GC/MS GC-ECD/FID GC/MS GC/MS 726 Appendix K Type/Class Method # Techniques Compounds CAS No Phenanthrene 85-01-8 Phenobarbital 50-06-6 Barbiturate 8270 GC/MS Phenol 108-95-2 Phenol 604 625 8040 8270 OLMO1 GC-FID/ECD GC/MS GC-ECD GC/MS GC/MS Phentermine (1,1-dimethyl-2phenyl ethanamine) 122-09-8 Aromatic amine 8270 GC/MS p-(Phenylazo) aniline (aminoazobenzene) 60-09-3 Aromatic amine 8270 GC/MS Phorate (Thimet) 298-02-2 Pesticide, organophosphorus 8140 8270 GC-FPD GC/MS Phosmet (Imidan) 732-11-6 Pesticide, organophosphorus 8270 GC/MS Phosphamidon (Dimecron) 13171-21-6 Pesticide, organophosphorus 8270 GC/MS Phthalic anhydride 85-44-9 Acid anhydride 8270 GC/MS Picloram 1918-02-1 Pesticide, chlorinated 515.1 GC-ECD 2-Picoline (2-methylpyridine) 109-06-8 Pyridine 8270 GC/MS Piperonyl sulfoxide 120-62-7 Sulfoxide 8270 GC/MS Prometon 1610-18-0 Pesticide, triazine 507 GC-NPD Pronamide 23950-58-5 Amide 515.1 GC-ECD n-Propylbenzene 103-65-1 VOC (aromatic) 502.1 524.2 8260 GC-PID GC/MS GC/MS Propylthiouracil 51-52-5 Organosulfur compound 8270 GC/MS Pyrene 129-00-0 Polynuclear aromatic hydrocarbon 525 550.1 610 625 8310 8270 OLMO1 GC/MS HPLC-FL HPLC-FL GC/MS HPLC-FL GC/MS GC/MS Polynuclear aromatic hydrocarbon 525 550.1 610 625 8310 8270 OLMO1 GC/MS HPLC-FL HPLC-FL GC/MS HPLC-FL GC/MS GC/MS Pyridine 110-86-1 Pyridine 8270 GC/MS Quinone 106-51-4 Aromatic ketone 8270 GC/MS Resorcinol (1,3-benzenediol) 108-46-3 Phenol 8270 GC/MS Safrole (1,2-methylendioxy-4-allyl benzene) 94-59-7 Aromatic 8270 GC/MS Appendix K 727 Method # Techniques Compounds CAS No Type/Class Santox (EPN) 2104-64-5 Pesticide, organophosphorus 8270 GC/MS Silvex (2,4,5-TP) 93-72-1 Chlorophenoxy acid herbicide 515.1 8150 GC-ECD GC-ECD Simazine 122-34-9 Pesticide, triazine 505 507 525 GC-ECD GC-NPD GC/MS Stirofos (Rabon, tetrachlorvinphos) 22248-79-9 Pesticide, organophosphorus 507 8140 8270 GC-NPD GC-FPD GC/MS Strychnine sulfate 60-41-3 Alkaloid 8270 GC/MS Styrene (vinylbenzene) 100-42-5 VOC (aromatic) 502.2 524.2 602 624 8020 8260 OLMO1 GC-PID GC/MS GC-PID GC/MS GC-PID GC/MS GC/MS 2,4,5-T 93-76-5 Chlorophenoxy acid herbicide 515.1 8150 GC-ECD GC-ECD 2,3,7,8-TCDF (2,3,7,8-tetrachlorodibenzofuran) 51207-31-9 Dibenzofuran 8280 GC/MS Terbufos (Counter) 13071-79-9 Pesticide, organophosphorus 507 8270 GC-NPD GC/MS 1,2,4,5-Tetrachlorobenzene 95-94-3 8270 GC/MS 1,1,1,2-Tetrachloroethane 630-20-6 Halogenated hydrocarbon (VOC) 502.2 524.2 8260 GC-ELCD GC/MS GC/MS 1,1,2,2-Tetrachloroethane 79-34-5 VOC (halocarbon) 502.2 524.2 601 624 8260 OLMO1 GC-ELCD GC/MS GC-HSD GC/MS GC/MS GC/MS Tetrachloroethylene (perchloroethylene) 127-18-4 Halogenated hydrocarbon (VOC) 502.2 524.2 601 624 8260 OLMO1 GC-ELCD GC/MS GC-HSD GC/MS GC/MS GC/MS Tetrachlorophenol 25167-83-3 Phenol 8040 GC-FID Tetraethylpyrophosphate (TEPP) 107-49-3 Organic phosphate 8270 GC/MS Thiophenol (benzenethiol, phenyl mercaptan) 108-98-5 Mercaptan 8270 GC/MS 728 Appendix K Compounds CAS No Toluene 108-88-3 Type/Class Aromatic Method # 502.2 524.2 602 624 8020 8260 Techniques GC-PID GC/MS GC-PID GC/MS GC-PID GC/MS Toluene-2,4-diisocyanate 584-84-9 Organic isocyanate 8270 GC/MS o-Toluidine 95-53-4 Aromatic amine 8270 GC/MS Toxaphene (Camphechlor) 8001-35-2 Pesticide, chlorinated 505 508 525 608 625 8080 8270 OLMO1 GC-ECD GC-ECD GC/MS GC-ECD GC/MS GC-ECD GC/MS GC/MS 1,2,3-Trichlorobenzene 87-61-6 VOC (halocarbon) 502.2 GC-ELCD/ PID GC/MS GC/MS 524.2 8260 1,2,4-Trichlorobenzene 120-82-1 Halogenated, aromatic 502.2 524.2 612 625 8120 8260 8270 OLMO1 GC-ELCD/ PID GC/MS GC-ECD GC/MS GC-ECD GC/MS GC/MS GC/MS 1,1,1-Trichloroethane (methyl chloroform) 71-55-6 Halocarbon 601 624 8260 OLMO1 GC-HSD GC/MS GC/MS GC/MS 1,1,2-Trichloroethane 79-00-5 VOC (halocarbon) 502.2 524.2 601 624 8260 OLMO1 GC-ELCD GC/MS GC-HSD GC/MS GC/MS GC/MS Trichloroethene 79-01-6 VOC (halocarbon) 502.2 GC-ELCD/ PID GC/MS GC-HSD GC/MS GC/MS GC/MS 524.2 601 624 8260 OLMO1 Appendix K Type/Class 729 Method # Techniques Compounds CAS No Trichlorofluoromethane (CFC-11) 75-69-4 VOC (halocarbon) 502.2 524.2 601 8260 GC-ELCD GC/MS GC-HSD GC/MS (Trichloromethyl) benzene 98-07-7 Chlorinated hydrocarbon 8120 GC-ECD Trichloronate 327-98-0 Pesticide, organophosphorus 8140 GC-FPD 2,4,5-Trichlorophenol 95-95-4 Phenol 8270 OLMO1 GC/MS GC/MS 2,4,6-Trichlorophenol 88-06-2 Phenol 604 625 8040 8270 OLMO1 GC-ECD/FID GC/MS GC-ECD/FID GC/MS GC/MS Trichlorophenol 25167-82-2 Phenol 8040 GC-FID 1,2,3-Trichloropropane 96-18-4 VOC (halocarbon) 502.2 524.2 8260 GC-ELCD GC/MS GC/MS O,O,O-Triethylphosphorothioate 126-68-1 Pesticide, organophosphorus 8270 GC/MS Trifluralin (Treflan) 1582-09-8 Pesticide, organofluorine 508 8270 GC-ECD GC/MS 2,4,5-Trimethylaniline 137-17-7 Aromatic amine 8270 GC/MS 1,2,4-Trimethylbenzene 95-63-6 Aromatic 502.2 524.2 8260 GC-PID GC/MS GC/MS Trimethylphosphate 512-56-1 Organic phosphate 8270 GC/MS 1,3,5-Trinitrobenzene 99-35-4 Nitroaromatic 8270 GC/MS Trithion (carbofenothion) 786-19-6 Pesticide, organophosphorus 8270 GC/MS Vancide-89 133-90-4 Pesticide, chlorinated 515.1 GC-ECD Vinyl chloride (chloroethene) 75-01-4 VOC (halocarbon) 502.2 524.2 GC-PID/ ELCD GC/MS 601 624 8260 OLMO1 GC-HSD GC/MS GC/MS GC/MS 531.1 HPLC-FL 1.1,2-Trichloro-1,2,2trifluoroethane (Freon-113) Vydate (Oxamyl) 23135-22-0 Pesticide, thiocarbamate 730 Appendix K Type/Class Method # Techniques Compounds CAS No m-Xylene 108-38-3 Aromatic 502.2 524.2 8260 GC-PID GC/MS GC/MS o-Xylene 95-47-6 Aromatic 502.2 524.2 8260 GC-PID GC/MS GC/MS p-Xylene 106-42-3 VOC (aromatic) 502.2 524.2 8260 GC-PID GC/MS GC/MS Xylenes (total xylene) 1330-20-7 Aromatic 8020 OLMO1 GC-PID GC/MS Zinophos (Thionazin) 297-97-2 Pesticide, organophosphorus 8270 GC/MS