Methods that have been developed for the analysis of polychlorinated biphenyls (PCBs) in used insulating oil are not usually applicable to the analysis of PCBs in waste oil. This method (EPA Victoria Method Number 6013) is to serve specifically as a method for the analysis of PCBs in waste oil. The method is applicable to the determination of commercial mixtures of PCBs in hydrocarbon based waste oils using gas chromatography (GC) with capillary columns.