USGS-NWQL: O-3104: Organochlorine and organophosphorous compounds, total recoverable

Summary
Analytes
Revision
Data and Sites

Official Method Name

Organochlorine and organophosphorous compounds, total recoverable, gas chromatographic

Current Revision

1983

Media

WATER

Instrumentation

Gas Chromatography with Electron Capture Detection

Method Subcategory

Organic

Method Source

USGS-NWQL

Citation

Methods for the Determination of Organic Substances in Water and Fluvial Sediments, Techniques of Water-Resources Investigations of the United States Geological Survey, Book 5, Chapter A3 Edited by R.L. Wershaw, M.J. Fishman, R.R Grabbe, and L.E. Lowe

Brief Method Summary

Organochlorine and organophosphorous compounds are extracted from approximately one liter of water or water suspended-sediment mixtures with hexane. Organophosphorous compounds are determined on a gas chromatograph with flame photometric detectors. The extracts are then purified using adsorption chromatography on an alumina column. If PCB's, PCN's, and toxaphene are present, the extracts are further purified using a silica gel column. The organochlorine compounds are then determined by gas chromatography using electron capture detectors.

Scope and Application

This method is suitable for the determination of organochlorine insecticides, polychlorinated biphenyls (PCB's), polychlorinated naphthalenes (PCN's), and organophosphorous insecticides in water and water-suspended-sediment mixtures containing at least 0.01 ug/L of the analyte.

Applicable Concentration Range

0.01 ug/L - 0.6 ug/L (undiluted)

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

Reagent water blank for each batch of samples. Calibrate daily with two point calibration.

Sample Handling

Description: 1 L Glass bottle, amber
Treatment and Preservation: Bottle baked at 4^oC by laboratory. DO NOT RINSE BOTTLE. Do not fill bottle beyond shoulder, as reagents must be added to the sample at the laboratory before analyses. Chill sample and maintain at 4^oC; ship immediately.

Maximum Holding Time

Seven days from collection to extraction.

Relative Cost

$201 to $400

Sample Preparation Methods

This method has 24 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	0.010 ug/L	67% Rec (SL)	13.00 % RSD (SL)
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	125% Rec (SL)	19.00 % RSD (SL)
Aldrin(309-00-2) Aldrex Aldrin Aldrin-R Aldrite Aldrosol HHDN Hexachlorohexahydro-endo-exo-dimethanonaphthalene Octalene Seedrin liquid	0.010 ug/L	89% Rec (SL)	17.00	0.01 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	0.100 ug/L	69% Rec (SL)	13.00	0.09 ug/L
Diazinon(333-41-5) Alfa-tox Basudin Diazide, Diazinone, Diazitol, Diazol Diazinon Diazinon (ANSI) Diazitol Dimpylate Dipofene Spectracide	0.010 ug/L	65% Rec (SL)	20.00	0.23 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	0.010 ug/L	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	0.010 ug/L	71% Rec (SL)	9.00	0.02 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	0.010 ug/L	N/A	N/A
Ethion(563-12-2) Bladan Diethion Ethion Ethodan Ethyl methylene phosphorodithioate Nialate O,O,O',O'-Tetraethyl S,S'-methylene bis( ... Tetraethyl S,S'-methylene bis(phosphorodithioate), O ... bis(S-(Diethoxyphosphinothioyl)mercapto)methane	0.010 ug/L	80% Rec (SL)	7.40 % RSD (SL)	0.15 ug/L
Ethyl parathion(56-38-2) DNTP Diethyl 4-nitrophenylphosphorothioate Diethyl-p-nitro phenyl mono thiophosphate Ethyl parathion Ethylparathion Niran O,O-Diethyl-O-p-nitrophenylphosphorothioate Parathion Parathion [phosphoric acid, O,O-diethyl-O-(4- ... Parathion ethyl Parathion, ethyl Parathion-ethyl Phosphorothioic acid, O,O-diethyl O-(4-nitroph Phosphorothioic acid, O,O-diethyl O-(4-nitrophenyl)ester	0.010 ug/L	80% Rec (SL)	6.30	0.15 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	0.010 ug/L	70% Rec (SL)	15.00	0.01 ug/L
Heptachlor epoxide(1024-57-3) Heptachlor epoxide Velsicol 53-CS-17 Vesicol 53-CS-17	0.010 ug/L	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	0.010 ug/L	86% Rec (SL)	12.00	0.01 ug/L
Malathion(121-75-5) Carbethoxy malathion Carbofos Cythion Dicarboethoxyethyl-o,o-dimethyl phosphorodithioate Malamar 50 Malathion Phosphothion Phosphothion, Sumitox Succinic acid, mercapto-, diethyl ester, S-est Sumitox	0.010 ug/L	69% Rec (SL)	32.00	0.26 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	0.010 ug/L	73% Rec (SL)	8.50	0.02 ug/L
Methyl parathion(298-00-0) Dimethylparathion Metacide Metaphos Methyl parathion Nitrox-80 O,O-dimethyl O-p-nitrophenyl phosphorothioate Parathion methyl Parathion, Methyl Parathion-methyl	0.010 ug/L	73% Rec (SL)	9.20	0.22 ug/L
Methyl trithion(953-17-3) Carbophenothion-Methyl Methyl carbophenothion Methyl trithion Trithion-methyl	0.010 ug/L	47% Rec (SL)	12.00	0.15 ug/L
Mirex(2385-85-5) Bichlorendo Cyclopentadiene,hexachloro-, dimer Dechlorane Ferriamicide Hexachloropentadiene dimer Mirex	0.010 ug/L	60% Rec (SL)	34.00	0.02 ug/L
Organochlorine pesticides(E-12851) Organochlorine pesticides Pesticides, organochlorine	N/A	N/A	N/A
Organophosphate pesticides(E-12873) Organophosphate pesticides Organophosphorus pesticides Pesticides, organophosphate	N/A	N/A	N/A
PCBs(1336-36-3) 1,1'-Biphenyl, chloro derivs. Aroclors PCB PCBs Polychlorinated biphenyl Polychlorinated biphenyl, NOS Polychlorinated biphenyls Polychlorobiphenyl	0.010 ug/L	58% Rec (SL)	28.00	0.12 ug/L
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	0.100 ug/L	32% Rec (SL)	9.40	0.12 ug/L
Toxaphene(8001-35-2) Alltox Camphechlor Camphechlor, Camphene, octachloro- Camphochlor Estonox Geniphene Phenacide Phenatox Polychlorocamphene Toxaphene Toxaphene ( Technical chlorinated camphene (67-69% ...	1.000 ug/L	N/A	N/A
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	0.010 ug/L	62% Rec (SL)	19.00 % RSD (SL)

Precision Descriptor Notes:
Detection Level Note:	Determination of organochlorine insecticides, polychlorinated biphenyls (PCBs), polychlorinated naphthalenes (PCNs), and organophosphorous insecticides in water and water-suspended sediment mixtures containing at least 0.01 ug/L of analyte.

Revision	PDF/Link
1983

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USGS-NWQL: O-3104: Organochlorine and organophosphorous compounds, total recoverable

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