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View Actual EPA Method 1668B (PDF File)
EPA Method 1668B:Chlorinated Biphenyl Congeners in Water, Soil, Sediment, Biosolids, and Tissue by HRGC/HRMS
Summary: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.
Scope: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).