Journal
TALANTA
Volume 59, Issue 4, Pages 673-680Publisher
ELSEVIER SCIENCE BV
DOI: 10.1016/S0039-9140(02)00580-5
Keywords
X-ray fluorescence spectrometry; energy dispersive; wear metals; used engine oil; inductively coupled plasma atomic emission spectrometry; microwave digestion
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A simple, particle size-independent spectrometric method has been developed for the multi-element determination of wear metals in used engine oil. A small aliquot (0.5 ml) of an acid-digested oil sample is spotted onto a G 18 solid phase extraction disk to form a uniform thin film. The dried disk is then analyzed directly by energy dispersive X-ray, fluorescence spectrometry. This technique provides a homogeneous and reproducible sample surface to the instrument, thus overcoming the typical problems associated with uneven particle size distribution and sedimentation. As a result, the method provides higher precision and accuracy than conventional methods. Furthermore, the disk sample may be stored and re-analyzed or extracted at a later date. The signals arising from the spotted disks, and the calibration curves constructed from them, are stable for at least 2 months. The limits of detection for Fe, Cu, Zn, Pb, and Cr are 5, 1, 4, 2, and 4 mug g(-1), respectively. Recoveries of these elements from spiked oil samples range from 92 to 110%. The analysis of two standard reference materials and a used oil sample produced results comparable to those found by inductively coupled plasma atomic emission spectrometry. (C) 2002 Elsevier Science B.V. All rights reserved.
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