Liquid chromatography–hydride generation–atomic fluorescence spectrometry hybridation for antimony speciation in environmental samples

Atomic fluorescence spectrometry was used as an element-specific detector in hybridation with liquid chromatography (LC) and hydride generation for the speciation of Sb(III), Sb(V) and trimethylantimony dichloride (TMSbCl2). The three species were poorly resolved in a single chromatogram but good results were obtained by anion-exchange chromatography, using a mobile phase with 20 mM EDTA and 8 mM hydrogenphthalate to separate Sb(III) and Sb(V) and 1 mM carbonate at pH 10 to separate Sb(V) and TMSbCl2. Calibration graphs were linear between 2 and 100 μg l−1. Detection limits were 0.9, 0.5 and 0.7 μg l−1 for Sb(III), Sb(V) and TMSbCl2, respectively. The method was applied to the speciation of antimony in environmental samples.