An extraction technique, involving homogenization of a sediment sample with dichloromethane at dual pH and phase separation by centrifugation, was used in the determination of fifty-one organic priority pollutants as identified in a standard reference sediment sample. The extract containing the base/neutral compounds was fractionated by gel permeation chromatography (GPC). Separation and identification of individual compounds in the silica gel fractions was accomplished by gas chromatography/mass spectrometry (GC/MS). Method precision and accuracy are discussed. Tentative identifications of other organic compounds found in the sediment are given.