Simultaneous determination of chromium (III) and chromium (VI) by reversed-phase ion-pair HPLC with chromium-specific detection

Abstract

A method for the simultaneous determination of Cr(III) and Cr(VI) with reversed-phase ion-pair HPLC employing chromium-specific detection by flame atomic absorption spectrometry (FAAS) and inductively-coupled plasma mass spectrometry (ICP-MS) is presented. Experimental parameters of the chromatographic separation, such as concentration of the ion-pairing reagent, pH and polarity of the mobile phase have been optimized for two different ion-pairing reagents, tetrabutylammonium phosphate (TBA) and tetraethylammonium nitrate (TEA). Best chromatographic conditions have been obtained with a polymer-based reversed-phase column (Hamilton PRP1) and mobile phases containing either TBA (1 mmol/l) in methanol-water (60:40, v/v) or TEA (2 mmol/l) in water at a pH between 3 and 4. With FAAS the detection limits (3σ) have been found to be 24 μg/l for Cr(III) and 40 μg/l for Cr(VI). A detection limit of 0.3 μg/l Cr(3σ) for both chromium species has been obtained when ICP-MS has been used for detection. The method has been applied to analyze tap- and groundwater and to investigate the behaviour of Cr(III) and Cr(VI) in spiked tap-water, as well as to analyze aqueous extracts of coal fly ash (NIST SRM 1633a) and of an ash from a wood treatment company.