Separation, preconcentration and speciation of chromium by solid phase extraction on immobilised ferron

Abstract

A sensitive and simple method for determination of chromium species after separation and preconcentration by solid phase extraction (SPE) has been developed. For the determination of the total concentration of chromium in solution, Cr(VI) was efficiently reduced to Cr(III) by addition of hydroxylamine and Cr(III) was preconcentrated on a column of immobilised ferron on alumina. The adsorbed analyte was then eluted with 5 mL of hydrochloric acid and was determined by flame atomic absorption spectrometery. The speciation of chromium was affected by first passing the solution through an acidic alumina column which retained Cr(VI) and then Cr(III) was preconcentrated by immobilised ferron column and determined by FAAS. The concentration of Cr(VI) was determined from the difference of concentration of total chromium and Cr(III). The effect of pH, concentration of eluent, flow rate of sample and eluent solution, and foreign ions on the sorption of chromium (III) by immobilised ferron column was investigated. Under the optimised conditions the calibration curve was linear over the range of 2–400 µg L−1 for 1000 mL preconcentration volume. The detection limit was 0.32 µg L−1, the preconcentration factor was 400, and the relative standard deviation (%RSD) was 1.9% (at 10 µg L−1; n = 7). The method was successfully applied to the determination of chromium species in water samples and total chromium in standard alloys.