Abstract An efficient method was developed for the determination of metals in used lubricating oils, by atomic absorption spectrometry. Oil samples were treated with an acid mixture and then emulsified in water (10% w/w) using ethoxy nonylphenol (6% w/w) as surfactant. Emulsion characteristics (oil, surfactant content and acid mixture) were optimized to obtain the best AAS signal. Good agreement was found between calibration curves of aqueous and emulsified standard solutions when a peristaltic pump was used to introduce the solutions into the flame. The emulsion methodology was comparable, within 95% of confidence, to traditional ashing methodologies when a standard reference oil and a used lubricating oil were analyzed. Precision between 0.4 and 5% RSD was obtained when real sample was analyzed using emulsions.