Simultaneous determination of Cr(iii) and Cr(vi) using reversed-phased ion-pairing liquid chromatography with dynamic reaction cell inductively coupled plasma mass spectrometry

Abstract

A method for the simultaneous determination of Cr(III) and Cr(VI) species in waters, soil leachates and synthetic bio-fluids is described. The method uses reversed-phase ion-pairing liquid chromatography to separate the chromium species and a dynamic reaction cell (DRC^®) equipped ICP-MS for detection of chromium. Separation of the chromium species is carried out in less than 2 min. Cr(III) is complexed with ethylenediaminetetraacetic acid (EDTA) prior to separation by mixing samples with the mobile phase containing 2.0 mM tetrabutylammonium hydroxide (TBAOH), 0.5 mM EDTA (dipotassium salt), and 5% (vol/vol) methanol, adjusted to pH 7.6. The interfering ⁴⁰Ar¹²C⁺ background peak at mass 52 was reduced by over four orders of magnitude to less than 200 cps by using 0.65 mL min⁻¹ ammonia as a reaction gas and an RPq setting on the DRC of 0.75. Method detection limits (MDLs) of 0.09 μg L⁻¹ for Cr(III) and 0.06 μg L⁻¹ for Cr(VI) were obtained based on peak areas at mass 52 for 50 μL injections of low level spikes. Reproducibility at 2 μg L⁻¹ was 3% RSD for 5 replicate injections. The tolerance of the method to various levels of common cations and anions found in natural waters and to matrix constituents found in soil leachates and simulated gastric and lung fluids was tested by performing spike recovery calculations for a variety of samples.