EPA Method 505


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EPA Method 505:
Analysis of Organohalide Pesticides and Commercial Polychlorinated Biphenyl (PCB) Products in Water by Microextraction and Gas Chromatography - Revision 2.1.

Summary:
A 35-mL sample is extracted with 2-mL of hexane. The concentrations of pesticides and PCBs in the extract are measured using a gas chromatography (GC) system equipped with a linearized electron capture detector (ECD).

Scope:
This method determines organochlorine pesticides and polychlorinated biphenyls (PCBs) in finished drinking water, drinking water during intermediate stages of treatment, and the raw source water.

Citation:
Methods for the Determination of Organic Compounds in Drinking Water - Supplement III (EPA/600/R-95-131)

Interferences:
(A) Glassware contamination: Thoroughly clean glassware, including baking or solvent rinse.(B) Reagent contamination: Use high purity reagents.(C) Contamination from sample carryover: Rinsing apparatus with hexane and purging equipment between analyses can minimize contamination.(D) Extracted interferences: Interference from extracted non-target compounds, with retention times similar to target compounds, can be reduced by cleaning the extract or using confirmation analysis.(E) Variable solvents: Use the same solvent for each analysis.(F) Endrin degradation: The splitless injector may cause endrin degradation. Endrin can break down by reacting with the active sites on the port sleeve.(G) PCBs loss to glass surfaces: Rinse glass and minimize sample contact with glass to prevent adsorption loss of PCBs.(H) Oxidation of target compounds: Oxidation of compounds (specifically easily-oxidized aldrin, hexachlorocyclopentadiene, and methoxychlor) can be prevented by adding sodium thiosulfate at collection.(I) Phthalate interference: An unknown interference (possibly dibutyl phthalate) appears in heptachlors retention window.

QC Requirements:
Initial demonstration of laboratory capability, followed by analysis of laboratory reagent blanks (LRB), laboratory fortified blanks (LFB), laboratory fortified sample matrix (LFM), and quality control samples (QCS). A MDL for each analyte must also be determined.

Maximum Holding Time:
14 days before extraction, except for heptachlor (7 days). Extracts up to 24 hours.

Media:
WATER

Subcategory:
Organic

Concentration:
Ranges differ for each analyte depending on matrix and instrumentation.

Precision:
Precision and accuracy values were calculated using data from five to eight analyses of fortified reagent water. NOTE: "PCBs" is a regulatory parameter in drinking water regulations, and encompasses the sum of multiple Aroclors. See performance data for specific Aroclors.

Detection:
MDLs were determined using the standard deviation of 5 to 8 replicate analyses of an analyte-fortified reagent water sample multiplied by the t-value for (# of samples - 1) degrees of freedom at the 99% confidence level. Detailed instructions for how MDLs are determined are found at 40 CFR part 136, Appendix B.

Revision Number:
Revision 2.1, 1995

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