A method applicable for the determination of 19 organochlorine (OC) pesticides, including total toxaphene as a complex mixture, and 3 polychlorinated biphenyl (PCB) mixtures as Aroclor equivalents--Aroclor 1016/1242, 1254, and 1260--in soil, aquatic bottom sediment, and suspended sediment is described. Method performance data are presented. The solvent system is designed to extract simultaneously selected OC pesticides and PCBs from the same sample matrix. The compounds are extracted by conventional Soxhlet extraction with dichloromethane, followed by partial isolation using gel permeation chromatography (GPC) to remove inorganic sulfur and large naturally present molecules from the sediment extract. The aliquot of extract collected from the GPC for OCs (OC pesticides and PCBs) is split into two sample fractions by alumina/silica combined-column chromatography, followed by Florisil adsorption chromatography to remove interfering compounds in the second fraction. The OC fractions are analyzed by dual capillary-column gas chromatography with electron-capture detection (GC/ECD). This report is limited to the determination of selected OC pesticides and PCBs by GC/ECD using this method. Interim reporting levels (IRLs) have been set at 0.400 to 3.12 micrograms per kilogram for 18 individual OC pesticides, 200 micrograms per kilogram for toxaphene, and 4.04 to 4.68 micrograms per kilogram for the PCBs, based on a sample size of 25-gram equivalent dry weight. These reporting levels may change following additional determinations of method detection limits.