EPA Method 608


ALS - Columbia offers EPA Method 608 testing at these laboratories:

Jacksonville Jacksonville, Florida Laboratory
Kelso Kelso, Washington Laboratory
Rochester Rochester, New York Laboratory

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EPA Method 608:
Organochlorine Pesticides and PCBs

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

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

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 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.

Maximum Holding Time:
Extract within 7 days of collection.Analyze within 40 days of extraction.

Media:
WATER

Subcategory:
Organic

Concentration:
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.

Sample Prep:
None.

Precision:
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:
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 Number:
40 CFR Part 136, Appendix A (Current Edition)

Test Description:
PCBs & Organochlorin

Instrument used for this test:
GC

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Examples:  8260
TO-15

Examples:  Dioxin
Mercury
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