The amount of acidic material in used engine oil is considered an indicator of the remaining useful life of the oil. Total acid number, determined by titration, is the most widely accepted method for determining acidic content but the method is not capable of speciation of individual acids. In this work, high molecular weight residue was isolated from used engine oil by dialysis in heptane. This residue was then analyzed using pyrolysis-comprehensive two dimensional gas chromatography with time-of-flight mass spectrometry. Carboxylic acids from C2-C18 were identified in the samples with acetic acid found to be the most abundant. This identification provides new information that may be used to improve the current acid detection methodologies for used engine oils.