Validation of an Analytical Procedure for Selected Polychlorinated Biphenyls Determination in Sediment Samples

this paper describes the method for determining 15 individual polychlorinated biphenyls in sediments, usingfexIkAextraction.�Theanalyticalprocedureincludedextractionandclean-upofextractswithcon- centratedsulfuricacidandsolidphaseextraction�(SPE)�onFlorisil.� Theidentificationandquantification� ofanalyteswerecarriedoutbycapillarygaschromatography�(GC)�withelectroncapturedetector�(ECD)� and/or low resolution mass spectrometry (lrMs). the method detection and quantification limits varied from 0.06 to 0.12 and from 0.2 to 0.4 ng/g dry weight, respectively. the relative standard deviations in repeatability and intra-laboratory reproducibility studies varied from 3.2 to 11.2%. recoveries of analytes from spiked sediment samples were between 74.0% and 108.8%. the method was linear and characterized bygoodcorrelationcoefficients�(>0.99)�forallcompoundsstudied.�Thequalityofthemethodundervalida - tionwasverifiedbytheanalysisofcertifiedreferencematerialandbyparticipationinaninterlaboratory� exercise.