Publicação: Determination of zinc in lubricating oil by flame AAS employing ultrasonic extraction
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The determination of zinc in lubricating oils by line-source flame atomic absorption spectrometry (LS-FAAS) is proposed employing an alternative sample preparation procedure based on ultrasonic wave-assisted acid extraction. The chemometric optimization of the main parameters influencing the extraction provided the following conditions: 1.3 mL of HCl, 5.0 mL of H2O 2, 120 seconds sonication time, 60 °C heating temperature, and 45% sonication amplitude of the ultrasound probe. Analytical curves in the 0.5-4.0 mg L-1 Zn range were consistently obtained (R= 0.9990). Commercial unused lubricating oil samples were analyzed by the proposed method and by high-resolution continuum source flame AAS (HR-CS FAAS) as the comparative technique. A paired t-test showed that the results between the two techniques were in agreement at the 95% confidence level. The accuracy of the proposed method was evaluated using an alternative sample preparation method based on recovery tests. Recoveries in the 92-119% interval were found. The relative standard deviation was 4% and the limit of detection was 17.6 μg L-1.
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Atomic Spectroscopy, v. 32, n. 6, p. 240-245, 2011.
