Chromium Speciation in Water by Sorption on Calcite and Determination by Electrothermal Atomic Absorption Spectrometry

Abstract

A rapid, sensitive, and accurate method for the separation and speciative determination of chromium (Cr)(VI) and Cr(III) in water samples has been developed using sorption as the separation technique in conjunction with final determination by electrothermal atomic absorption spectroscopy (ETAAS). The present method, where granular calcite is used as selective sorbent, separates Cr(III) with retention values up to 99%, resulting in high accuracy determination of Cr(VI). Total Cr was likewise determined by ETAAS after an efficient reduction of Cr(VI) to Cr(III) using ascorbic acid as reducing agent, deriving Cr(III) concentration from the difference between total Cr and Cr(VI). The parameters of the separation technique, solution pH (4.5–5.5), solution flow rate through the calcite column (0.14–0.42 mL min^?1), and calcite column internal diameter (1.5–3.0 cm), were evaluated. Best results were achieved with pH of 5.5, flow rate of 0.42 mL min^?1, and column internal diameter of 1.5 cm. Optimum determination conditions were found using magnesium nitrate Mg(NO₃)₂] as chemical modifier, pyrolysis, and atomization temperatures of 1400 and 2200°C, respectively. In such conditions, the detection limits (n=10) were 1.5 and 0.8 µg L^?1 for Cr(III) and Cr(VI), respectively.