EPA Method 1668B

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EPA Method 1668B:
Chlorinated Biphenyl Congeners in Water, Soil, Sediment, Biosolids, and Tissue by HRGC/HRMS

Aqueous samples (samples containing less than one percent solids)-Stable isotopically labeled analogs of the Toxics and labeled LOC CBs are spiked into a 1-L sample. The sample is extracted using solid-phase extraction (SPE), separatory funnel extraction (SFE), or continuous liquid/liquid extraction (CLLE). Solid, semi-solid, and multi-phase samples (excluding tissue)-The labeled compounds are spiked into a sample containing 10 g (dry weight) of solids. Samples containing multiple phases are pressure filtered and any aqueous liquid is discarded. Coarse solids are ground or homogenized. Any non-aqueous liquid from multi-phase samples is combined with the solids and extracted in a Soxhlet/Dean-Stark (SDS) extractor. The extract is concentrated for cleanup. Fish and other tissue-A 20-g aliquot of sample is homogenized, and a 10-g aliquot is spiked with the labeled compounds. The sample is mixed with anhydrous sodium sulfate, allowed to dry for 12 - 24 hours, and extracted for 18-24 hours using methylene chloride in a Soxhlet extractor. The extract is evaporated to dryness, and the lipid content is determined.

Method 1668B (the Method) is for determination of chlorinated biphenyl congeners (CBs) in wastewater and other matrices by high resolution gas chromatography/high resolution mass spectrometry (HRGC/HRMS).