Simple and Fast Two-Step Fully Automated Methodology for the Online Speciation of Inorganic Antimony Coupled to ICP-MS

A very simple, fast and non-chromatographic methodology for inorganic antimony speciation based on Multisyringe Flow Injection Analysis (MSFIA) employing online hydride generation (HG) ICP-MS was developed. The fully automated analysis is performed in two steps: firstly, Sb(III) is quantified by ICP-MS after chemical vapor generation; then, total antimony is determined in the presence of potassium iodide as a pre-reducer of Sb(V) to Sb(III). The Sb(V) concentration is quantified by the difference between the total antimony and Sb(III) concentrations, reaching an analysis frequency of 30 h−1. The optimization was performed using a Box Behnken design. The MSFIA-HG-ICP-MS system allows the antimony speciation analysis with a detection limit of 0.016 µg L−1 for Sb(III), working in a linear range of 0.053 to 5.0 µg L−1. This method was applied for the determination of Sb(III) and Sb(V) in water samples from Maiorca Island, Spain, and the concentrations found varied from 0.10 to 0.14 µg L−1 for Sb(III) and from 0.12 to 0.28 µg L−1 for Sb(V). The results were validated by addition/recovery tests, obtaining recoveries between 90 and 111% in both cases. Furthermore, a good precision was achieved, 1.4% RSD, and sample and reagent consumption were reduced to a few mL, with the consequent decrease in waste generation. Thus, the proposed method is a good tool for the speciation of inorganic antimony at ultra-trace levels in waters, allowing its risk assessment