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Method Summary

Method Source U.S. EPA Engineering and Analysis Division
Method Number608
Revision Information40 CFR Part 136, Appendix A (Current Edition)
Method NameDescriptive Name: Organochlorine Pesticides and PCBs via GC with Electron Capture Detector (ECD)

Official Name: Organochlorine Pesticides and PCBs

MediaMedia: WATER
SubcategoryOrganic
Citation EPA Method Guidance CD-ROM (includes MCAWW Methods, and most current EPA Methods)
Method Download Adobe Acrobat (pdf) icon Download full method now (PDF file)
Summary of MethodA 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 ApplicationThis 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 Range4xMDL 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.
QC RequirementsInitial 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 HandlingSamples 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 4oC from time of collection to time of extraction.
Max Holding TimeExtract within 7 days of collection.
Analyze within 40 days of extraction.
Relative Cost/Effort$201 to $400
Sample Prep Method(s)None.
 

Method Organochlorine Pesticides and PCBs via GC with Electron Capture Detector (ECD) has 26 analytes associated with it.

Analyte


Detection
Level

Bias Precision Pct False
Positive
Organochlorine pesticides
(E-12851)		N/AN/AN/A 
4,4'-DDD
(72-54-8)		.011 ug/L114 % Rec (ML)15 % RSD (ML)1 ug/L
Endosulfan-II
(33213-65-9)		.004 ug/L127 % Rec (ML)31 % RSD (ML)1 ug/L
Endosulfan-I
(959-98-8)		.014 ug/L101 % Rec (ML)26 % RSD (ML)1 ug/L
Toxaphene
(8001-35-2)		.24 ug/L254 % Rec (ML)29 % RSD (ML)1 ug/L
Heptachlor
(76-44-8)		.003 ug/L73 % Rec (ML)27 % RSD (ML)1 ug/L
Endrin aldehyde
(7421-93-4)		.023 ug/LN/AN/A1 ug/L
4,4'-DDE
(72-55-9)		.004 ug/L99 % Rec (ML)19 % RSD (ML)1 ug/L
Endrin
(72-20-8)		.006 ug/L85 % Rec (ML)53 % RSD (ML)1 ug/L
Dieldrin
(60-57-1)		.002 ug/L92 % Rec (ML)33 % RSD (ML)1 ug/L
Lindane
(58-89-9)		.004 ug/L77 % Rec (ML)27 % RSD (ML)1 ug/L
Chlordane
(57-74-9)		.014 ug/L78 % Rec (ML)41 % RSD (ML)1 ug/L
PCB-1242
(53469-21-9)		.065 ug/L96.5 % Rec (ML)29 % RSD (ML)20 ug/L
p,p'-DDT
(50-29-3)		.012 ug/L80 % Rec (ML)5 % RSD (ML)1 ug/L
delta-BHC
(319-86-8)		.009 ug/L88 % Rec (ML)28 % RSD (ML)1 ug/L
beta-BHC
(319-85-7)		.006 ug/L88 % Rec (ML)27 % RSD (ML)1 ug/L
alpha-BHC
(319-84-6)		.003 ug/L87 % Rec (ML)23 % RSD (ML)1 ug/L
Aldrin
(309-00-2)		.004 ug/L85 % Rec (ML)19 % RSD (ML)1 ug/L
PCB-1016
(12674-11-2)		N/A83.5 % Rec (ML)18 % RSD (ML)20 ug/L
PCB-1248
(12672-29-6)		N/A102.3 % Rec (ML)23 % RSD (ML)20 ug/L
PCB-1232
(11141-16-5)		N/A144.95 % Rec (ML)43 % RSD (ML)20 ug/L
PCB-1221
(11104-28-2)		N/A99.25 % Rec (ML)32 % RSD (ML)20 ug/L
PCB-1254
(11097-69-1)		N/A86.35 % Rec (ML)38 % RSD (ML)20 ug/L
PCB-1260
(11096-82-5)		N/A84.8 % Rec (ML)10 % RSD (ML)20 ug/L
Endosulfan sulfate
(1031-07-8)		.066 ug/L52 % Rec (ML)91 % RSD (ML)1 ug/L
Heptachlor epoxide
(1024-57-3)		.083 ug/L99 % Rec (ML)17 % RSD (ML)1 ug/L
export_analytes
Precision Descriptor NotesThe 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 NoteMDL 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.
 
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