EPA-OGWDW/TSC: 508.1: Chlorinated Pesticides, Herbicides, and Organohalides in Water by GCECD

Summary
Analytes
Revision
Data and Sites

Official Method Name

Determination of Chlorinated Pesticides, Herbicides, and Organohalides by Liquid-Solid Extraction and Electron Capture Gas Chromatography

Current Revision

Revision 2.0, 1995

Media

WATER

Instrumentation

Gas Chromatography with Electron Capture Detection

Method Subcategory

Organic

Method Source

EPA-OGWDW/TSC

Citation

Methods for the Determination of Organic Compounds in Drinking Water - Supplement III (EPA/600/R-95-131)

Brief Method Summary

A 1-L sample is passed through a liquid/solid extraction (LSE) disk or cartridge containing a solid inorganic matrix coated with a chemically bonded C-18 organic phase. The analytes (pesticides, herbicides, and organohalides) are eluted from the LSE disk or cartridge with small volumes of ethyl acetate and methylene chloride, and this eluate is concentrated by evaporation of some of the solvent. The concentrations of analytes are determined using a fused silica capillary column gas chromatography (GC) system equipped with an electron capture detector (ECD).

NOTE: CAS Numbers in NEMI for cis- and trans- permethrin differ from those in the method. The CAS Numbers in NEMI are the correct ones.

Scope and Application

This method determines 29 chlorinated pesticides, three herbicides, and four organohalides in drinking water, ground water, and drinking water in any treatment stage.

Applicable Concentration Range

Ranges differ for each analyte depending on matrix and instrumentation.

Interferences

(A) Reagent contamination: Use high purity reagents.

(B) Contamination from sample carryover: Rinsing apparatus replacing syringes and injection port liners as needed can minimize contamination.

Quality Control Requirements

Initial demonstration of laboratory capability, followed by laboratory reagent blanks (LRBs), laboratory fortified blanks (LFBs), and laboratory fortified matrix samples. Additional quality control practices are recommended. Initial demonstration of capability is demonstrated by analysis of a minimum of four replicate LFBs containing each analyte of concern at a suggested concentration in the range of 0.01 - 0.5 ug/L. The mean accuracy should be 70% to 130% and the RSD should be less than 30%. A method detection limit (MDL) must also be determined for each analyte.

Sample Handling

Dechlorinate samples by adding 50 mg/L of sodium sulfite. Adjust the sample to a pH less than 2 by adding up to 4 mL of 6N HCl. Sample should be kept sealed from collection until analysis. Sampling equipment must not use plastic tubing, plastic gaskets, or any parts that may leach interfering analytes into the sample. Store samples at 4^oC until analysis.

NOTE: Samples collected for cyanazine determination MUST NOT be dechlorinated or acidified when collected. Acidification and dechlorination must occur immediately prior to fortification with surrogate standard and extraction.

Maximum Holding Time

14 days.

Relative Cost

$201 to $400

Sample Preparation Methods

This method has 51 analytes associated with it.

Analyte	Detection Level	Bias	Precision	Spiking Level
4,4'-DDD(72-54-8) 1,1-Dichloro-2,2-bis(p-chlorophenyl)ethane 4,4'-DDD Benzene, 1,1'-(2,2-dichloroethylidene)bis[4-ch Benzene, 1,1'-(2,2-dichloroethylidene)bis[4-chloro- Dichloro-2,2-bis(p-chlorophenyl)ethane,1,1- Dichlorodiphenyldichloroethane Ethane, 1,1-dichloro-2,2-bis(p-chlorophenyl)- Rhothane TDE Tetrachlorodiphenylethane p,p'-DDD p,p'-Dichlorodiphenyl dichloroethane p,p'-TDE	0.003 ug/L	90% Rec (SL)	8.89 % RSD (SL)	0.01 ug/L
4,4'-DDE(72-55-9) 1,1'-(-Dichloroethenylidene)bis(4-chlorobenzene) 4,4'-DDE 4,4'-DDE, DDT, DDD Benzene, 1,1'-(dichloroethenylidene)bis[4-chlo Benzene, 1,1'-(dichloroethenylidene)bis[4-chloro- Ethylene, 1,1-dichloro-2,2-bis(p-chlorophenyl)- bis(p-Chlorophenyl)-1,1-dichloroethylene,2,2- p,p'-DDE p,p'-Dichlorodiphenyldichloroethylene	0.003 ug/L	80% Rec (SL)	11.20 % RSD (SL)	0.01 ug/L
Alachlor(15972-60-8) 2-Chloro-N-(2,6-diethylphenyl)-N-(methoxymethy Acetanilide,2-chloro-2',6'-diethyl-n-(methoxymethyl)- Alachlor Alanex Lasso Metachlor Methachlor	0.009 ug/L	80% Rec (SL)	37.50 % RSD (SL)	0.01 ug/L
Aldrin(309-00-2) Aldrex Aldrin Aldrin-R Aldrite Aldrosol HHDN Hexachlorohexahydro-endo-exo-dimethanonaphthalene Octalene Seedrin liquid	0.009 ug/L	80% Rec (SL)	37.50 % RSD (SL)	0.01 ug/L
Atrazine(1912-24-9) 1,3,5-Triazine-2,4-diamine, 6-chloro-N-ethyl-N'-(1- ... 2-Chloro-4-(ethylamino)-6-(isopropylamino)-S-triazine 2-Chloro-4-(ethylamino)-6-(isopropylamino)-s-t 2-Chloro-4-ethylamino-6-isopropylamine-sym-triazine AAtrex Atratol 8P Atrazine Atrazine (ANSI) Bicep	0.003 ug/L	140% Rec (SL)	7.14 % RSD (SL)	0.01 ug/L
Biopermethrin(51877-74-8) (+)-trans-Permethrin Biopermethrin	0.007 ug/L	110% Rec (SL)	20.00 % RSD (SL)	0.01 ug/L
Butachlor(23184-66-9) 2-Chloro-2',6'-diethyl-N-(butoxymethyl)acetanilide Acetamide, N-(butoxymethyl)-2-chloro-N-(2,6-di Acetanilide,2-chloro-2',6'-diethyl-n-(butoxymethyl)- Butachlor Butachlor (ANSI) Butanox Hiltachlor Machete N-(Butoxymethyl)-2-chloro-N-(2,6-diethylphenyl)acetamide N-(butoxymethyl)-2-chloro-2',6'-diethyl acetan N-(butoxymethyl)-2-chloro-2',6'-diethyl acetanilide	0.070 ug/L	86% Rec (SL)	5.50 % RSD (SL)	0.50 ug/L
Chlordane(57-74-9) Chlordane Chlordane, .alpha.,.beta., and .gamma. isomers Chlorindan Compound K (FDA) Corodane Octachloro-4,7-methanotetrahydroindane Toxichlor Velsicol 1068	N/A	N/A	N/A
Chlorobenzilate(510-15-6) 4,4'-Dichlorobenzilic acid ethyl ester Acaraben Benzeneacetic acid, 4-chloro-alpha-(4-chloroph Benzeneacetic acid, 4-chloro-alpha-(4-chlorophenyl)- ... Benzilan Benzilic acid, 4,4'-dichloro-, ethyl ester Chlorobenzilate ECB Ethyl-2-hydroxy-2,2-bis(4-chlorophenyl) acetate Ethyl-4,4'-dichlorobenzilate Folbex	0.002 ug/L	80% Rec (SL)	8.75 % RSD (SL)	0.01 ug/L
Chloroneb(2675-77-6) 1,4-Dichloro-2,5-dimethoxybenzene Chloroneb Demosan Dichloro-2,5-dimethoxybenzene,1,4- Terraneb B Terraneb SP	0.006 ug/L	120% Rec (SL)	15.80 % RSD (SL)	0.01 ug/L
Chlorothalonil(1897-45-6) 1,3-Benzenedicarbonitrile, 2,4,5,6-tetrachloro 1,3-Benzenedicarbonitrile, 2,4,5,6-tetrachloro- 2,4,5,6-Tetrachloro-1,3-dicyanobenzene 2,4,5,6-Tetrachloroisophthalonitrile Bravo Chloroalonil Chlorothalonil Daconil 2787 Isophthalonitrile, tetrachloro- Sweep Vanox	0.002 ug/L	70% Rec (SL)	10.00 % RSD (SL)	0.01 ug/L
Cyanazine(21725-46-2) 2-((4-Chloro-6-(ethylamino)-1,3,5-triazin-2-yl)amino)-2-methylpropanenitrile 2-((4-Chloro-6-(ethylamino)-s-triazin-2-yl)amino)-2-methylpropionitrile Bladex Cyanazine Fortrol Payze	0.007 ug/L	100% Rec (SL)	22.00 % RSD (SL)	0.01 ug/L
DCPA(1861-32-1) Chlorothal Chlorthaldimethyl DCPA Dacthal Dimethyl tetrachloroterephthalate Dimethyl-2,3,5,6-tetrachlorotephthalate Tetrachloroterephthalic acid, dimethyl ester	0.009 ug/L	100% Rec (SL)	28.00 % RSD (SL)	0.01 ug/L
Dieldrin(60-57-1) 1,2,3,4,10,10-Hexachloro-6,7-epoxy-1,4,4a,5, 6 1,2,3,4,10,10-Hexachloro-6,7-epoxy-1,4,4a,5, 6,7,8, ... 2,7:3,6-Dimethanonaphth(2,3-b)oxirene, 3,4,5,6 2,7:3,6-Dimethanonaphth(2,3-b)oxirene, 3,4,5,6,9,9- ... Alvit Dieldrin Dieldrin (hexachloroepoxyoctahydro-endo,exo- ... Dieldrin/aldrin Dimethanonaphthalene, 1,2,3,4,10,10-hexachloro-6,7- ... Heod Octalox	0.003 ug/L	70% Rec (SL)	12.90 % RSD (SL)	0.01 ug/L
Endosulfan sulfate(1031-07-8) 6,9-Methano-2,3,4-benzodioxathiepin, 6,7 Benzoepin sulfate Endosulfan sulfate Hexachloro-5-norbornene-2,3-dimethanol,1,4,5,7,7-, ... Thiodan sulfate	0.003 ug/L	70% Rec (SL)	14.30 % RSD (SL)	0.01 ug/L
Endosulfan-I(959-98-8) 6,9-Methano-2,4,3-benzodioxathiepin, 6,7,8,9,10,10- ... Endosulfan-I Endosulfan-alpha Thiodan I alpha-Endosulfan	0.006 ug/L	70% Rec (SL)	27.10 % RSD (SL)	0.01 ug/L
Endosulfan-II(33213-65-9) AI3-29022 CCRIS 1461 Endosulfan B Endosulfan II Endosulfan-II Endosulfan-beta Thiodan II beta-Benzoepin beta-Endosulfan	0.001 ug/L	70% Rec (SL)	42.90 % RSD (SL)	0.01 ug/L
Endrin(72-20-8) 2,7:3,6-Dimethanonaphth[2,3-b]oxirene, 3,4,5,6,9,9- ... 3,4,5,6,9,9-Hexachloro-1a,2,2a,3,6,6a,7,7a-oct 3,4,5,6,9,9-Hexachloro-1a,2,2a,3,6,6a,7,7a-octahydro ... Compound 269 Endrin Hexachloroepoxyoctahydro-endo,endo-dimethanonaphthalene Hexadrin Mendrin Nendrin	0.007 ug/L	150% Rec (SL)	15.30 % RSD (SL)	0.01 ug/L
Endrin aldehyde(7421-93-4) 1,2,4-Methenocyclopenta[c,d]pentalene-5- ... Endrin aldehyde	0.004 ug/L	80% Rec (SL)	15.00 % RSD (SL)	0.01 ug/L
Etridiazole(2593-15-9) 1,2,4-Thiadiazole, 5-ethoxy-3-(trichloromethyl 1,2,4-Thiadiazole, 5-ethoxy-3-(trichloromethyl)- 5-Ethoxy-3-(trichloromethyl)-1,2,4-thiadiazole ETMT Ethazol Ethoxy-3-trichloromethyl-1,2,4-thiadiazole,5- Etridiazole Koban Terrazole Truban	0.010 ug/L	110% Rec (SL)	40.90 % RSD (SL)	0.01 ug/L
Heptachlor(76-44-8) 1,4,5,6,7,8,8-Heptachlorotetrahydro-4,7-methanoindene Drinox Heptachlor Heptachlor [1,4,5,6,7,8,8-heptachloro-3a,4,7,7a- ... Heptachlor/Heptachlor epoxide (SARA 110) Heptachlorodicyclopentadiene Heptagran Heptamul Velsicol-104	0.005 ug/L	90% Rec (SL)	17.80 % RSD (SL)	0.01 ug/L
Heptachlor epoxide(1024-57-3) Heptachlor epoxide Velsicol 53-CS-17 Vesicol 53-CS-17	0.001 ug/L	60% Rec (SL)	5.00 % RSD (SL)	0.01 ug/L
Herbicides(E-12839) Herbicide formulations Herbicides	N/A	N/A	N/A
Hexachlorobenzene(118-74-1) Anticarie Benzene, hexachloro- Bunt-cure HCB Hexachlorobenzene Perchlorobenzene	0.001 ug/L	100% Rec (SL)	4.00 % RSD (SL)	0.01 ug/L
Hexachlorocyclopentadiene(77-47-4) 1,3-Cyclopentadiene, 1,2,3,4,5,5-hexachloro- HCCPD HCP Hexachloro-1,3-cyclopentadiene Hexachlorocyclo-1,3-pentadiene Hexachlorocyclopentadiene Perchlorocyclopentadiene	0.004 ug/L	40% Rec (SL)	32.50 % RSD (SL)	0.01 ug/L
Lindane(58-89-9) Cyclohexane, 1,2,3,4,5,6-hexachloro-, (1-alpha Cyclohexane, 1,2,3,4,5,6-hexachloro-, (1-alpha, 2- ... HCH-gamma Hexachlorocyclohexane (gamma) Lindane Lindane ( gamma isomer of benzene hexachloride ) (99 ... gamma-BHC gamma-Benzenehexachloride gamma-HCH gamma-Hcch gamma-Hexachlorocyclohexane	0.006 ug/L	70% Rec (SL)	28.60 % RSD (SL)	0.01 ug/L
Methoxychlor(72-43-5) 1,1'-(2,2,2-Trichloroethylidene)bis[4-methoxybenzene] 1,1,1-Trichloro-2,2-bis(4-methoxyphenyl)ethane Benzene, 1,1'-(2,2,2-trichloroethylidene)bis[4-methoxy- Dimethoxy DDT Ethane, 1,1,1-trichloro-2,2-bis(p-methoxypheny Ethane, 1,1,1-trichloro-2,2-bis(p-methoxyphenyl)- Marlate Methoxcide Methoxychlor Metox p,p'-Methoxychlor p,p'DMDT	0.003 ug/L	60% Rec (SL)	15.00 % RSD (SL)	0.01 ug/L
Metolachlor(51218-45-2) 2-Chloro-N-(2-ethyl-6-methylphenyl)-N-(2-methoxy-4- ... 2-Chloro-N-(6-ethyl-o-tolyl)-N-(2-methoxy-1- ... 2-chloro-6'-ethyl-N-(2-methoxy-1-methylethyl)-o- ... Acetamide, 2-chloro-N-(2-ethyl-6-methylphenyl)-N-(2- ... Codal Cycle Dual Metelilachlor Metolachlor Metolachlor (ANSI)	0.015 ug/L	113% Rec (SL)	18.20 % RSD (SL)	0.03 ug/L
Metribuzin(21087-64-9) 4-Amino-6-(1,1-dimethylethyl)-3-(methylthio)-1 Bay 94337 Lexone Metribuzin Sencoral Sencorer	0.009 ug/L	90% Rec (SL)	31.10 % RSD (SL)	0.01 ug/L
Organics, semivolatile(E-12884) Organics, semivolatile Semi-volatile organics Semivolatile organics	N/A	N/A	N/A
Organochlorine pesticides(E-12851) Organochlorine pesticides Pesticides, organochlorine	N/A	N/A	N/A
PCB-1016(12674-11-2) Aroclor 1016 PCB-1016	0.029 ug/L	82% Rec (SL)	5.70 % RSD (SL)	0.20 ug/L
PCB-1221(11104-28-2) Aroclor 1221 PCB-1221	0.037 ug/L	85% Rec (SL)	6.80 % RSD (SL)	0.20 ug/L
PCB-1232(11141-16-5) Aroclor 1232 PCB-1232	0.033 ug/L	90% Rec (SL)	5.80 % RSD (SL)	0.20 ug/L
PCB-1242(53469-21-9) Arochlor 1242 Aroclor 1242 PCB-1242	0.043 ug/L	100% Rec (SL)	6.90 % RSD (SL)	0.20 ug/L
PCB-1248(12672-29-6) Aroclor 1248 Biphenyl, tetrachloro- PCB-1248	0.044 ug/L	88% Rec (SL)	8.00 % RSD (SL)	0.20 ug/L
PCB-1254(11097-69-1) Arochlor 1254 Aroclor 1254 PCB-1254	0.036 ug/L	82% Rec (SL)	7.00 % RSD (SL)	0.20 ug/L
PCB-1260(11096-82-5) Arochlor 1260 Aroclor 1260 PCB-1260	0.012 ug/L	82% Rec (SL)	2.40 % RSD (SL)	0.20 ug/L
PCBs(1336-36-3) 1,1'-Biphenyl, chloro derivs. Aroclors PCB PCBs Polychlorinated biphenyl Polychlorinated biphenyl, NOS Polychlorinated biphenyls Polychlorobiphenyl	N/A	N/A	N/A
Propachlor(1918-16-7) 2-Chloro-N-isopropylacetanilide 2-Chloro-n-isopropyl-n-phenylacetamide Acetamide, 2-chloro-N-(1-methylethyl)-N-phenyl Acetamide, 2-chloro-N-(1-methylethyl)-N-phenyl- Bexton Propachlor Propachlore Ramrod	0.008 ug/L	80% Rec (SL)	33.80 % RSD (SL)	0.01 ug/L
Simazine(122-34-9) 1,3,5-Triazine-2,4-diamine, 6-chloro-N,N'-diethyl- 2,4-bis(Ethylamino)-6-chloro-s-triazine 2-Chloro-4,6-bis(ethylamino)-1,3,5-triazine 2-Chloro-4,6-bis(ethylamino)-S-triazine 6-Chloro-N,N'-diethyl-1,3,5-triazine-2,4-diami 6-Chloro-N,N'-diethyl-1,3,5-triazine-2,4-diamine Aquazine Princep Radocon S-Triazine,2-chloro-4,6-bis(ethylamino)- Simadex, Simanex, Simazine (ANSI) Simazine	0.008 ug/L	90% Rec (SL)	27.80 % RSD (SL)	0.01 ug/L
Toxaphene(8001-35-2) Alltox Camphechlor Camphechlor, Camphene, octachloro- Camphochlor Estonox Geniphene Phenacide Phenatox Polychlorocamphene Toxaphene Toxaphene ( Technical chlorinated camphene (67-69% ...	0.130 ug/L	81% Rec (SL)	5.10 % RSD (SL)	1.00 ug/L
Trifluralin(1582-09-8) Commence Dinitro-n,n-dipropyl-4-(trimethylfluoro)benzenamine,2,6- Treflan Trifluoralin, Trifluraline Trifluralin Triflurex p-Toluidine, alpha, alpha, alpha-trifluoro-2,6	0.001 ug/L	60% Rec (SL)	5.00 % RSD (SL)	0.01 ug/L
alpha-BHC(319-84-6) .alpha.-Benzenehexachloride Cyclohexane, 1,2,3,4,5,6-hexachloro-, alpha-isomer HCH-alpha alpha-BHC alpha-HCH alpha-Hexachlorocyclohexane alpha-Lindane	0.001 ug/L	70% Rec (SL)	42.80 % RSD (SL)	0.01 ug/L
alpha-Chlordane(5103-71-9) 4,7-Methano-1H-indene 1,2,4,5,6,7,8,8-octachlo Methanoindan, 1-alpha,2-alpha,4-beta,5,6,7-beta,8,8- ... Methanoindan,alpha-1,2,4,5,6,7,8,8-octachloro-3a- ... alpha-Chlordane cis-4,7-Methano-1H-indene 1,2,4,5,6,7,8,8-octachloro ... cis-Chlordane	0.004 ug/L	70% Rec (SL)	17.10 % RSD (SL)	0.01 ug/L
beta-BHC(319-85-7) Cyclohexane, 1,2,3,4,5,6-hexachloro-, beta-isomer HCH-beta beta-BHC beta-Benzenehexachloride beta-HCH beta-Hexachlorocyclohexane beta-Lindane	0.009 ug/L	90% Rec (SL)	32.20 % RSD (SL)	0.01 ug/L
cis-Permethrin(61949-76-6) Permethrin I cis-Permethrin	0.009 ug/L	70% Rec (SL)	42.90 % RSD (SL)	0.01 ug/L
delta-BHC(319-86-8) .delta.-Benzenehexachloride Cyclohexane, 1,2,3,4,5,6-hexachloro-, delta-isomer HCH-delta delta-BHC delta-HCH delta-Hexachlorocyclohexane delta-Lindane	0.004 ug/L	80% Rec (SL)	17.50 % RSD (SL)	0.01 ug/L
p,p'-DDT(50-29-3) 1,1,1-Trichloro-2,2-bis(p-chlorophenyl)ethane 4,4'-DDT Benzene, 1,1'-(2,2,2-trichloroethylidene)bis[4-chloro- Chlorophenothane DDT Dichlorodiphenyltrichloroethane Ethane, 1,1,1-trichloro-2,2-bis(p-chlorophenyl)- bis(p-Chlorophenyl)-2,2,2-trichloroethane,1,1- p,p'-DDT p,p'-Dichlorodiphenyltrichloroethane	0.004 ug/L	120% Rec (SL)	9.20 % RSD (SL)	0.01 ug/L
trans-Chlordane(5103-74-2) AI3-16398 EINECS 225-826-0 Methanoindan, 1,2,3,5,6,7,8,8-octachlor-3a,4,7,7a- ... Methanoindan,1,2,4,5,6,7,8,8-octachloro-3a,4,7,7a- ... trans-4,7-Methano-1H-indene 1,2,4,5,6,7,8,8- ... trans-Chlordan trans-Chlordane	0.001 ug/L	60% Rec (SL)	50.00 % RSD (SL)	0.01 ug/L
trans-Permethrin(61949-77-7) Permethrin II trans-Permethrin	0.007 ug/L	110% Rec (SL)	20.00 % RSD (SL)	0.01 ug/L

Precision Descriptor Notes:	Precision and accuracy values determined using single laboratory data from seven replicate measurements of reagent water sample fortified with the analytes of interest. NOTE: "PCBs" is a regulatory parameter in drinking water regulations, and encompasses the sum of multiple Aroclors. See performance data for specific Aroclors. NOTE: CAS Numbers in NEMI for cis- and trans- permethrin differ from those in the method. The CAS Numbers in NEMI are the correct ones.
Detection Level Note:	MDLs were determined using the standard deviation of 7 replicate analyses of an analyte-fortified reagent water sample multiplied by the t-value for 6 degrees of freedom at the 99% confidence level. Detailed instructions for how MDLs are determined are found at 40 CFR part 136, Appendix B.

Precision Descriptor Notes:

Precision and accuracy values determined using single laboratory data from seven replicate measurements of reagent water sample fortified with the analytes of interest. NOTE: "PCBs" is a regulatory parameter in drinking water regulations, and encompasses the sum of multiple Aroclors. See performance data for specific Aroclors. NOTE: CAS Numbers in NEMI for cis- and trans- permethrin differ from those in the method. The CAS Numbers in NEMI are the correct ones.

Detection Level Note:

MDLs were determined using the standard deviation of 7 replicate analyses of an analyte-fortified reagent water sample multiplied by the t-value for 6 degrees of freedom at the 99% confidence level. Detailed instructions for how MDLs are determined are found at 40 CFR part 136, Appendix B.

Revision	PDF/Link
Revision 2.0, 1995

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EPA-OGWDW/TSC: 508.1: Chlorinated Pesticides, Herbicides, and Organohalides in Water by GCECD

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