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Under the provisions of the U. S. Toxic Substances Control Act,  the U. S. Environmental Protection Agency (EPA) has implemented rules for the handling and disposal of polychlorinated biphenyl-(PCB) contaminated insulating fluids.[2,3,4] To properly handle and dispose of oils, the EPA classifies electrical insulating fluids as non-PCB (0 to 50 ppm), PCB-contaminated (50 to 500 ppm), or PCB (greater than 500 ppm). An improved analysis method is presented for determining both qualitative and quantitative PCBs in insulating fluids. This method uses an acid wash, Florisil isolation of the PCBs from the oil, and capillary gas chromatography analysis.