EPA-RCA: 8081B: Organochlorine Pesticides by GC-ECD

Summary
Analytes
Revision
Data and Sites

Official Method Name

Organochlorine Pesticides by Gas Chromatography

Current Revision

Revision 2, November 2000

Media

VARIOUS

Instrumentation

Gas Chromatography with Electron Capture Detection

Method Subcategory

Organic

Method Source

EPA-RCA

Citation

SW-846 Update IVB

Brief Method Summary

A measured volume or weight of sample (approximately 1 L for liquids, 2 to 30 g for solids) is extracted using the appropriate matrix-specific sample extraction technique. A variety of cleanup steps may be applied to the extract, depending on the nature of the matrix interferences and the target analytes. Suggested cleanups include alumina (Method 3610), Florisil (Method 3620), silica gel (Method 3630), gel permeation chromatography (Method 3640), and sulfur (Method 3660). After cleanup, the extract is analyzed by injecting a measured aliquot into a gas chromatograph with either a narrow-bore or wide-bore fused-silica capillary column, and either an electron capture detector (GC/ECD) or an electrolytic conductivity detector (GC/ELCD).

Scope and Application

Method 8081 may be used to determine the concentrations of various organochlorine pesticides in extracts from solid and liquid matrices, using fused-silica, open-tubular, capillary columns with electron capture detectors (ECD) or electrolytic conductivity detectors (ELCD).

Applicable Concentration Range

None given.

Interferences

(1) Contamination of samples, solvent, and carrier gases with target analytes (especially compounds common to environmental laboratories, like methylene chloride).
(2) Contamination of samples with sulfur (primarily present in base-neutral fractions).
(3) Septum bleed (compounds from the injection septum are analyzed with the sample).
(4) Column bleed (compounds from column coating break down, decreasing column efficiency).
(5) Ghost peaks (compounds adsorb strongly to the column and carry over to later runs).
(6) Coelution of species.
(7) Coextracted contaminants.
(8) Phthalate esters interfere with detection of pesticides via electron capture detector.

Quality Control Requirements

(see ch.1, SW-846 Methods 3500, 8000), CV, calibration standard, initial demonstration of proficiency, MB, MS, MSD, LD, LCS, and the addition of surrogates to each field sample and QC sample, CS (after 20 samples)

Sample Handling

Store the extract in the refrigerator and analyze it within 40 days of extraction. See SW-846, Chapter 4, Organic Analytes, Section 4. See SW-846 Chapter Four for information.

Maximum Holding Time

Aqueous samples - 7 days (sample), 40 days (extract). Solid samples - 14 days (sample), 40 (extract). Also, see SW-846 Chapter Four for information.

Relative Cost

$201 to $400

Sample Preparation Methods

This method has 53 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	0.850 ug/L	57% Rec (SL)	11.00 % RSD (SL)	500.00 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	0.590 ug/L	52% Rec (SL)	11.00 % RSD (SL)	500.00 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	N/A	N/A	N/A
Aldrin(309-00-2) Aldrex Aldrin Aldrin-R Aldrite Aldrosol HHDN Hexachlorohexahydro-endo-exo-dimethanonaphthalene Octalene Seedrin liquid	0.830 ug/L	92% Rec (SL)	33.00 % RSD (SL)	500.00 ug/L
Biopermethrin(51877-74-8) (+)-trans-Permethrin Biopermethrin	N/A	N/A	N/A
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	N/A	N/A	N/A
Chloroneb(2675-77-6) 1,4-Dichloro-2,5-dimethoxybenzene Chloroneb Demosan Dichloro-2,5-dimethoxybenzene,1,4- Terraneb B Terraneb SP	N/A	N/A	N/A
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	N/A	N/A	N/A
DBCP(96-12-8) 1,2-Dibromo-3-chloropropane Chloro-1,2-dibromopropane,3- DBCP Dibromochloropropane Fumagon, Fumazone Nemabrom, Nemafume, Nemagon, Nematocide Nemagon Nematocide Propane, 1,2-dibromo-3-chloro-	N/A	N/A	N/A
DCPA(1861-32-1) Chlorothal Chlorthaldimethyl DCPA Dacthal Dimethyl tetrachloroterephthalate Dimethyl-2,3,5,6-tetrachlorotephthalate Tetrachloroterephthalic acid, dimethyl ester	N/A	N/A	N/A
Diallate(2303-16-4) 2,3-DCDT Avadex Diallate Diisopropylthiocarbamic acid, s-2,3-dichloroallyl ester S-(2,3-Dichloroallyl) diisopropyl-thiocarbamate	N/A	N/A	N/A
Dichlone(117-80-6) 1,4-Naphthalenedione, 2,3-dichloro- 1,4-Naphthoquinone, 2,3-dichloro- 2,3-Dichloro-1,4-naphthoquinone Dichlone Dichloro-1,4-naphthoquinone,2,3- Dichloronaphthquinone Phygon	N/A	N/A	N/A
Dicofol(115-32-2) 1,1-bis(Chlorophenyl)-2,2,2-trichloroethanol 4,4'-Dichloro-alpha-(trichloromethyl)-Benzhydrol 4-Chloro-alpha-(4-chlorophenyl)-alpha-( ... Acarin Benzenemethanol, 4-chloro-alpha-(4-chloropheny DTMC Di(p-chlorophenyl)-trichloromethylcarbinol Dicofol Kelthane Kelthane, Mitigan p,p'-Dicofol	N/A	N/A	N/A
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	N/A	89% Rec (SL)	19.00 % RSD (SL)	500.00 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	N/A	N/A	N/A
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	0.510 ug/L	52% Rec (SL)	11.00 % RSD (SL)	500.00 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	0.540 ug/L	52% Rec (SL)	10.00 % RSD (SL)	500.00 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	0.820 ug/L	56% Rec (SL)	10.00 % RSD (SL)	500.00 ug/L
Endrin aldehyde(7421-93-4) 1,2,4-Methenocyclopenta[c,d]pentalene-5- ... Endrin aldehyde	0.360 ug/L	45% Rec (SL)	6.00 % RSD (SL)	500.00 ug/L
Endrin ketone(53494-70-5) 2,5,7-Metheno-3H-cyclopenta[a]pentalen-3-one, 3b,4,5 ... Endrin ketone Keto-endrin	N/A	N/A	N/A
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	N/A	N/A	N/A
Halowax 1000(58718-66-4) Halowax 1000	N/A	N/A	N/A
Halowax 1001(58718-67-5) Halowax 1001	N/A	N/A	N/A
Halowax 1013(12616-35-2) Halowax 1013	N/A	N/A	N/A
Halowax 1014(12616-36-3) Halowax 1014	N/A	N/A	N/A
Halowax 1099(39450-05-0) Halowax 1099	N/A	N/A	N/A
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	0.560 ug/L	60% Rec (SL)	13.00 % RSD (SL)	500.00 ug/L
Heptachlor epoxide(1024-57-3) Heptachlor epoxide Velsicol 53-CS-17 Vesicol 53-CS-17	0.340 ug/L	54% Rec (SL)	11.00 % RSD (SL)	500.00 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	N/A	N/A	N/A
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	N/A	N/A	N/A
Isodrin(465-73-6) 1,2,3,4,10,10-Hexachloro-1,4,4a,5,8,8a-hexahyd 1,2,3,4,10,10-Hexachloro-1,4,4a,5,8,8a-hexahydro-1,4 ... Compound 711 Dimethanonaphthalene, 1,2,3,4,10,10-hexachloro-1,4,, ... Hexachlorohexahydro-endo,endo-dimethanonaphtha Hexachlorohexahydro-endo,endo-dimethanonaphthalene Isodrin	N/A	N/A	N/A
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	0.320 ug/L	55% Rec (SL)	9.00 % RSD (SL)	500.00 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	N/A	N/A	N/A
Mirex(2385-85-5) Bichlorendo Cyclopentadiene,hexachloro-, dimer Dechlorane Ferriamicide Hexachloropentadiene dimer Mirex	N/A	N/A	N/A
Nitrofen(1836-75-5) 2,4-Dichloro-1-(4-nitrophenoxy)benzene 2,4-Dichlorophenyl-p-nitrophenylether Benzene, 2,4-dichloro-1-(4-nitrophenoxy)- Ether, 2,4-dichlorophenyl p-nitrophenyl- Nitrofen TOK	N/A	N/A	N/A
Octachloronaphthalene(2234-13-1) Halowax 1051 Naphthalene, octachloro- Octachloronaphthalene Perchloronaphthalene	N/A	N/A	N/A
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
Pentachloronitrobenzene(82-68-8) Benzene, pentachloronitro- Brassicol PCNB Pentachloronitrobenzene Quintozene Terrachlor Terraclor Terracur	N/A	N/A	N/A
Perthane(72-56-0) 1,1-Dichloro-2,2-bis(4-ethylphenyl) ethane 1,1-Dichloro-2,2-bis(ethylphenyl)ethane 1,1-Dichloro-2,2-bis(p-ethylphenyl)ethane Benzene, 1,1'-(2,2-dichloroethylidene)bis[4-ethyl- Dichloro-1,1-bis(p-ethylphenyl)ethane,2,2- Diethyl diphenyl dichloroethane and related compounds Ethylan Perthane p,p-ethyl-DDD	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	N/A	N/A	N/A
Strobane(8001-50-1) Dichloricide Aerosol Strobane Strobane (R) Terpene polychlorinates* consists of chlorinated ...	N/A	N/A	N/A
Toxaphene(8001-35-2) Alltox Camphechlor Camphechlor, Camphene, octachloro- Camphochlor Estonox Geniphene Phenacide Phenatox Polychlorocamphene Toxaphene Toxaphene ( Technical chlorinated camphene (67-69% ...	N/A	N/A	N/A
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	N/A	N/A	N/A
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	N/A	88% Rec (SL)	25.00 % RSD (SL)	500.00 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	0.580 ug/L	49% Rec (SL)	8.00 % RSD (SL)	500.00 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	0.200 ug/L	351% Rec (SL)	71.00 % RSD (SL)	500.00 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	0.350 ug/L	51% Rec (SL)	11.00 % RSD (SL)	500.00 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	0.710 ug/L	57% Rec (SL)	10.00 % RSD (SL)	500.00 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	0.580 ug/L	50% Rec (SL)	9.00 % RSD (SL)	500.00 ug/L
trans-Nonachlor(39765-80-5) trans-Nonachlor	N/A	N/A	N/A

Precision Descriptor Notes:	NOTE: SPIKING CONCENTRATION FOR PRECISION AND ACCURACY IS IN UNITS OF NANOGRAMS per GRAM (ng/g). Precision and accuracy data was obtained using three replicate analyses of a sewage sludge spiked with 500 to 1000 ng/g of analyte. Sample clean-up was performed using ultrasonic extraction (see SW-846 Method 3550). The method contains additional performance information obtained with Soxhlet Extraction and Solid Phase Extraction.
Detection Level Note:	MDLs were determined using a solid phase extraction preparation (SW-846 Method 3535) through the analysis of 7 spiked wastewater replicates.

Precision Descriptor Notes:

NOTE: SPIKING CONCENTRATION FOR PRECISION AND ACCURACY IS IN UNITS OF NANOGRAMS per GRAM (ng/g). Precision and accuracy data was obtained using three replicate analyses of a sewage sludge spiked with 500 to 1000 ng/g of analyte. Sample clean-up was performed using ultrasonic extraction (see SW-846 Method 3550). The method contains additional performance information obtained with Soxhlet Extraction and Solid Phase Extraction.

Detection Level Note:

MDLs were determined using a solid phase extraction preparation (SW-846 Method 3535) through the analysis of 7 spiked wastewater replicates.

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Revision 2, November 2000

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EPA-RCA: 8081B: Organochlorine Pesticides by GC-ECD

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