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Khuhawar MY, Arain GM: Liquid chromatographic determination of vanadium in petroleum oils and mineral ore samples using 2-acetylpyridne-4-phenyl-3-thiosemicarbazone as derivatizing reagent. Talanta. 2006 Jan 15;68(3):535-41. Epub 2005 Jun 20.
Liquid chromatographic method has been developed, based on precolumn derivatization of vanadium (V) with 2-acetylpyridine-4-phenyl-3-thiosemicarbazone (APPT). The complex is extracted in chloroform together with palladium (II), tin (II) and iron (III) and eluted and separated completely from Kromasil 100 C-18, 10mum (25cmx4.6mm i.d.) column with methanol:water:acetonitrile (60:30:10, v/v/v) with a flow rate of 1ml/min. UV detection was at 260nm. Linear calibration curve was obtained with 1-12.5mug/ml vanadium (V) with detection limit of 8ng/injection (20mul). A number of metal ions tested did not affect the determination of vanadium. The test mixtures were analyzed for vanadium (IV) and vanadium (V) contents and relative% error was obtained +/-1-8%. The method was applied for the determination of vanadium in petroleum oils and mineral ore samples with vanadium contents of 0.32-2.3 and 121.7-717.3mug/g with R.S.D. of 1.5-4.5 and 0.38-4.7%, respectively. The results correlated with reported values and by atomic absorption spectrophotometry. |
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