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Organic acid degradation products and other anions in engine oil were speciated by capillary electrophoresis (CE) and liquid chromatography-mass spectrometry (LCMS) with electrospray ionization. The sample preparation procedure involved selectively extracting the acids and other water soluble salts into 0.05M aqueous potassium hydroxide. Samples of engine-aged mineral oil and synthetic engine oil contained formic acid, acetic acid, and complex mixtures of fatty acid degradation products. CE analysis of formic acid, acetic acid and selected fatty acids is proposed as a new chemical analysis method for evaluating the condition of engine oil and for studying the effects of high temperature-high load (HTHL) oxidation. Because the overall pattern of CE peaks in the electropherogram changes with oil age or condition, CE-fingerprint (i.e., pattern recognition) techniques may also be useful for evaluating an aged oil's condition or remaining service life.