Speciation and preconcentration of inorganic antimony in waters by Duolite GT-73 microcolumn and determination by segmented flow injection-hydride generation atomic absorption spectrometry (SFI-HGAAS)

A selective matrix removal/separation/enrichment method, utilizing a microcolumn of a chelating resin with SH functional groups (Duolite GT-73), was proposed for the determination of Sb(III) in waters by segmented flow injection-hydride generation atomic absorption spectrometry (SFI-HGAAS). The resin was selective to Sb(III) at almost all pH and acidity values employed, whereas Sb(V) was not retained at all and could be determined after a pre-reduction step with l-cysteine. Spike recoveries were tested at various concentration levels in different water types and were found to vary between 85 and 118%. Accuracy of the proposed methodology was checked by analyzing a standard reference material and a good correlation was found between the determined (13.3 ± 1.1 μg l−1) and the certified value (13.79 ± 0.42 μg l−1). The method was applied to several bottled drinking water samples for antimony determination with and without preconcentration and none of the samples were found to contain antimony above the permissible level (5 μg l−1). The characteristic concentration (the concentration of the analyte corresponding to an absorbance of 0.0044) was 0.55 μg l−1 and the 3 s limit of detection (LOD) based on five times preconcentration was 0.06 μg l−1. The applicability of the microcolumn separation/preconcentration/matrix removal method for flow injection systems was also demonstrated.