Speciation analysis of inorganic antimony in sediment samples from São Paulo Estuary, Bahia State, Brazil

This paper proposes an extraction procedure for the speciation analysis of inorganic antimony in sediment samples using slurry sampling and hydride generation atomic absorption spectrometry. The optimization step of extraction of the species was performed employing a full two-level factorial design (2³) and a Box-Behnken matrix where the studied factors in both experiments were: extraction temperature, ultrasonic radiation time, and hydrochloric acid concentration. Using the optimized conditions, antimony species can be extracted in closed system using a 6.0 M hydrochloric acid solution at temperature of 70 °C and an ultrasonic radiation time of 20 min. The determination of antimony is performed in presence of 2.0 M hydrochloric acid solution using HG AAS by external calibration technique with limits of detection and quantification of 5.6 and 19.0 ng L⁻¹ and a precision expressed as relative standard deviation of 5.6 % for an antimony solution with concentration of 6.0 μg L⁻¹. The accuracy of the method was confirmed by analysis of two certified reference materials of sediments. For a sample mass of sediment of 0.20 g, the limits of detection and quantification obtained were 0.70 and 2.34 ng g⁻¹, respectively. During speciation analysis, antimony(III) is determined in presence of citrate, while total antimony is quantified after reduction of antimony(V) to antimony(III) using potassium iodide and ascorbic acid. The method was applied for analysis of six sediment samples collected in São Paulo Estuary (Bahia State, Brazil). The antimony contents obtained varied from 45.3 to 89.1 ng g⁻¹ for total antimony and of 17.7 to 31.4 ng g⁻¹ for antimony(III). These values are agreeing with other data reported by the literature for this element in uncontaminated sediment samples.