EPA-EAD: 608: Organochlorine Pesticides and PCBs via GC with Electron Capture Detector (ECD)

Summary
Analytes
Revision
Data and Sites

Official Method Name

Organochlorine Pesticides and PCBs

Current Revision

40 CFR Part 136, Appendix A (Current Edition)

Media

WATER

Instrumentation

Gas Chromatography with Electron Capture Detection

Method Subcategory

Organic

Method Source

EPA-EAD

Citation

EPA Method Guidance CD-ROM (includes MCAWW Methods, and most current EPA Methods)

Brief Method Summary

A 1L sample is extracted using a liquid/liquid phase extraction technique with methylene chloride as the extracting solvent. The extract is dried through sodium sulfate, exchanged to hexane, and then concentrated down to a volume of less than 10mL. The extract is then separated using gas chromatography with an ECD. Method 624 can be used for GC/MS confirmation of compound match or interference.

Scope and Application

This is a GC method where organochlorine pesticides and PCBs are detected from municipal and industrial discharges listed under 40 CFR part 136.1.

Applicable Concentration Range

4xMDL to 1000xMDL (ug/L), except for chlordane was low (60%) at 4xMDL and Toxaphene was demonstrated linear over a range of 10xMDL to 1000xMDL.

Interferences

(A) Glassware: Must be scrupulously cleaned. Prior to detergent washing, the glassware should be rinsed with the last solvent used and then placed in a muffle furnace to remove any thermally unstable organic compounds. Some thermally organic compounds, such as PCBs may still remain. A rinse with acetone or pesticide quality hexane may be substituted in place of the muffle furnace. Store glassware inverted or capped with aluminum foil.
(B) Contamination: Phthalate esters are commonly found in most products in the lab, since it is used as a plasticizer. Extra attention to cleaning of glassware is a must.
(C) Co-extraction: The extraction process will sometimes extract certain analytes that may cause possible interference with the target compounds. A Florisil cleanup procedure is described in Section 11 of the method.

Quality Control Requirements

Initial demonstration of laboratory capability and the periodic analysis of laboratory reagent blanks, fortified blanks, and other laboratory solutions as a continuing check on performance.

Sample Handling

Samples should be grabbed in 1 Liter or 1 Quart amber bottles with Teflon-lined cap. Store samples away from direct sunlight. The bottles must be washed, rinsed with methylene chloride or acetone, and dried before use to minimize contamination. Samples should be iced or kept refrigerated at 4^oC from time of collection to time of extraction.

Maximum Holding Time

Extract within 7 days of collection.
Analyze within 40 days of extraction.

Relative Cost

$201 to $400

Sample Preparation Methods

None.

This method has 26 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	0.011 ug/L	114% Rec (ML)	15.00 % RSD (ML)	1.00 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	0.004 ug/L	99% Rec (ML)	19.00 % RSD (ML)	1.00 ug/L
Aldrin(309-00-2) Aldrex Aldrin Aldrin-R Aldrite Aldrosol HHDN Hexachlorohexahydro-endo-exo-dimethanonaphthalene Octalene Seedrin liquid	0.004 ug/L	85% Rec (ML)	19.00 % RSD (ML)	1.00 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	0.014 ug/L	78% Rec (ML)	41.00 % RSD (ML)	1.00 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	0.002 ug/L	92% Rec (ML)	33.00 % RSD (ML)	1.00 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	0.066 ug/L	52% Rec (ML)	91.00 % RSD (ML)	1.00 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	0.014 ug/L	101% Rec (ML)	26.00 % RSD (ML)	1.00 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	0.004 ug/L	127% Rec (ML)	31.00 % RSD (ML)	1.00 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	0.006 ug/L	85% Rec (ML)	53.00 % RSD (ML)	1.00 ug/L
Endrin aldehyde(7421-93-4) 1,2,4-Methenocyclopenta[c,d]pentalene-5- ... Endrin aldehyde	0.023 ug/L	N/A	N/A	1.00 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	0.003 ug/L	73% Rec (ML)	27.00 % RSD (ML)	1.00 ug/L
Heptachlor epoxide(1024-57-3) Heptachlor epoxide Velsicol 53-CS-17 Vesicol 53-CS-17	0.083 ug/L	99% Rec (ML)	17.00 % RSD (ML)	1.00 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	0.004 ug/L	77% Rec (ML)	27.00 % RSD (ML)	1.00 ug/L
Organochlorine pesticides(E-12851) Organochlorine pesticides Pesticides, organochlorine	N/A	N/A	N/A
PCB-1016(12674-11-2) Aroclor 1016 PCB-1016	N/A	84% Rec (ML)	18.00 % RSD (ML)	20.00 ug/L
PCB-1221(11104-28-2) Aroclor 1221 PCB-1221	N/A	99% Rec (ML)	32.00 % RSD (ML)	20.00 ug/L
PCB-1232(11141-16-5) Aroclor 1232 PCB-1232	N/A	145% Rec (ML)	43.00 % RSD (ML)	20.00 ug/L
PCB-1242(53469-21-9) Arochlor 1242 Aroclor 1242 PCB-1242	0.065 ug/L	97% Rec (ML)	29.00 % RSD (ML)	20.00 ug/L
PCB-1248(12672-29-6) Aroclor 1248 Biphenyl, tetrachloro- PCB-1248	N/A	102% Rec (ML)	23.00 % RSD (ML)	20.00 ug/L
PCB-1254(11097-69-1) Arochlor 1254 Aroclor 1254 PCB-1254	N/A	86% Rec (ML)	38.00 % RSD (ML)	20.00 ug/L
PCB-1260(11096-82-5) Arochlor 1260 Aroclor 1260 PCB-1260	N/A	85% Rec (ML)	10.00 % RSD (ML)	20.00 ug/L
Toxaphene(8001-35-2) Alltox Camphechlor Camphechlor, Camphene, octachloro- Camphochlor Estonox Geniphene Phenacide Phenatox Polychlorocamphene Toxaphene Toxaphene ( Technical chlorinated camphene (67-69% ...	0.240 ug/L	254% Rec (ML)	29.00 % RSD (ML)	1.00 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	0.003 ug/L	87% Rec (ML)	23.00 % RSD (ML)	1.00 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	0.006 ug/L	88% Rec (ML)	27.00 % RSD (ML)	1.00 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	0.009 ug/L	88% Rec (ML)	28.00 % RSD (ML)	1.00 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	0.012 ug/L	80% Rec (ML)	5.00 % RSD (ML)	1.00 ug/L

Precision Descriptor Notes:	The precision and accuracy values were determined using regression equations derived from a 20 laboratory validation study. The study determined analytes using reagent water, drinking water, surface water, and three industrial wastewaters spiked at six concentrations. Concentrations used in this study ranged from 0.5 to 30 mg/L for single-component pesticides and from 8.5 to 400 ug/L for multi-component parameters. Single operator precision, overall precision, and accuracy were found to be directly related to the concentration of the parameter and essentially independent of the sample matrix.
Detection Level Note:	MDL procedure is equivalent to the procedure at 40 CFR part 136, Appendix B. MDLs were determined using the standard deviation of 7 replicate analyses of a analyte-fortified reagent water sample multiplied by the t-value for 6 degrees of freedom at the 99% confidence level (3.14). Detailed instructions for how MDLs are determined are found in Section 14 of the Method.

Precision Descriptor Notes:

The precision and accuracy values were determined using regression equations derived from a 20 laboratory validation study. The study determined analytes using reagent water, drinking water, surface water, and three industrial wastewaters spiked at six concentrations. Concentrations used in this study ranged from 0.5 to 30 mg/L for single-component pesticides and from 8.5 to 400 ug/L for multi-component parameters. Single operator precision, overall precision, and accuracy were found to be directly related to the concentration of the parameter and essentially independent of the sample matrix.

Detection Level Note:

MDL procedure is equivalent to the procedure at 40 CFR part 136, Appendix B. MDLs were determined using the standard deviation of 7 replicate analyses of a analyte-fortified reagent water sample multiplied by the t-value for 6 degrees of freedom at the 99% confidence level (3.14). Detailed instructions for how MDLs are determined are found in Section 14 of the Method.

Revision	PDF/Link
40 CFR Part 136, Appendix A (Current Edition)

The Water Quality Portal contains sample results from sites that use this method.

Download WQP data

Select data:

Sites only
Sample results only

File format:

Comma-separated
Tab-separated
MS Excel 2007+

Sites where this method was used

Loading Sites ...

EPA-EAD: 608: Organochlorine Pesticides and PCBs via GC with Electron Capture Detector (ECD)

WHO WE ARE

LEGAL