AOAC: 990.06: Organochlorine Pesticide in Water by GC

Summary
Analytes
Revision
Data and Sites

Official Method Name

Organochlorine Pesticides in Finished Drinking Water by Gas Chromatographic Method

Current Revision

Final Action - 1993

Media

WATER

Instrumentation

Gas Chromatography with Electron Capture Detection

Method Subcategory

Organic

Method Source

AOAC

Citation

Official Methods of Analysis of AOAC International, 16th Edition, 4th Revision, 1998 Volume I

Brief Method Summary

Measured volume of test portion (1 L) is extracted with CH2Cl2 by shaking in separatory funnel or mechanical tumbling in bottle. CH2Cl2 extract is separated, dried with anhydrous Na2SO4, solvent exchanged with methyl tert-butyl ether (MTBE), and concentrated to 5 mL. Pesticides are separated and measured by capillary column gas chromatography with electron-capture detection. Estimated method detection limits range from 0.0015 g/L for gamma-chlordane to 5 g/L for chlorobenzilate; values for 24 compounds range between 0.025 and 0.5 g/L.

Scope and Application

Applicable to the determination of 29 organochlorine pesticides in drinking water.

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

IDMP, MB, SS, instrument QC std.

Sample Handling

Glass collection bottles are prepared by adding preservative. Collect 1 L grab samples by conventional sampling practices. Refrigerate at 4 degrees C until extracted. Extract within 7 days of collection.

Maximum Holding Time

7 days

Relative Cost

$201 to $400

Sample Preparation Methods

This method has 31 analytes associated with it.

Analyte	Detection Level	Bias	Precision
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	N/A	15.10 % RSD (ML)
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	0.010 ug/L	N/A	16.60 % RSD (ML)
Aldrin(309-00-2) Aldrex Aldrin Aldrin-R Aldrite Aldrosol HHDN Hexachlorohexahydro-endo-exo-dimethanonaphthalene Octalene Seedrin liquid	0.070 ug/L	N/A	14.30 % RSD (ML)
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	5.000 ug/L	N/A	18.30 % RSD (ML)
Chloroneb(2675-77-6) 1,4-Dichloro-2,5-dimethoxybenzene Chloroneb Demosan Dichloro-2,5-dimethoxybenzene,1,4- Terraneb B Terraneb SP	0.500 ug/L	N/A	17.00 % RSD (ML)
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	0.020 ug/L	N/A	24.40 % RSD (ML)
DCPA(1861-32-1) Chlorothal Chlorthaldimethyl DCPA Dacthal Dimethyl tetrachloroterephthalate Dimethyl-2,3,5,6-tetrachlorotephthalate Tetrachloroterephthalic acid, dimethyl ester	0.020 ug/L	N/A	16.30 % RSD (ML)
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	0.020 ug/L	N/A	15.80 % RSD (ML)
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	0.010 ug/L	N/A	16.90 % RSD (ML)
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	0.010 ug/L	N/A	13.90 % RSD (ML)
Endosulfan-II(33213-65-9) AI3-29022 CCRIS 1461 Endosulfan B Endosulfan II Endosulfan-II Endosulfan-beta Thiodan II beta-Benzoepin beta-Endosulfan	0.010 ug/L	N/A	12.30 % RSD (ML)
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	0.020 ug/L	N/A	13.60 % RSD (ML)
Endrin aldehyde(7421-93-4) 1,2,4-Methenocyclopenta[c,d]pentalene-5- ... Endrin aldehyde	0.020 ug/L	N/A	12.40 % RSD (ML)
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	0.020 ug/L	N/A	15.90 % RSD (ML)
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	0.010 ug/L	N/A	12.30 % RSD (ML)
Heptachlor epoxide(1024-57-3) Heptachlor epoxide Velsicol 53-CS-17 Vesicol 53-CS-17	0.010 ug/L	N/A	12.70 % RSD (ML)
Herbicides(E-12839) Herbicide formulations Herbicides	N/A	N/A	N/A
Hexachlorobenzene(118-74-1) Anticarie Benzene, hexachloro- Bunt-cure HCB Hexachlorobenzene Perchlorobenzene	0.008 ug/L	N/A	13.70 % RSD (ML)
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	0.010 ug/L	N/A	N/A
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	0.050 ug/L	N/A	18.80 % RSD (ML)
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
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	0.500 ug/L	N/A	13.40 % RSD (ML)
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	0.020 ug/L	N/A	14.80 % RSD (ML)
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	0.020 ug/L	N/A	13.80 % RSD (ML)
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	0.002 ug/L	N/A	13.80 % RSD (ML)
cis-Permethrin(61949-76-6) Permethrin I cis-Permethrin	0.500 ug/L	N/A	14.60 % RSD (ML)
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	0.010 ug/L	N/A	12.40 % RSD (ML)
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	0.060 ug/L	N/A	14.00 % RSD (ML)
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	0.002 ug/L	N/A	13.10 % RSD (ML)
trans-Permethrin(61949-77-7) Permethrin II trans-Permethrin	0.500 ug/L	N/A	27.60 % RSD (ML)

Precision Descriptor Notes:	Precision and accuracy data reflect multilaboratory method performance in reagent water. Note: Data in the method does not specify the concentration dependence of the stated precision.
Detection Level Note:	Estimated MDLs from Table 990.06B of the method.

Revision	PDF/Link
Final Action - 1993

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AOAC: 990.06: Organochlorine Pesticide in Water by GC

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