Speciation of dissolved inorganic antimony in natural waters using liquid phase semi-microextraction combined with electrothermal atomic absorption spectrometry

Abstract Liquid–liquid extraction preconcentration technique which allows the achievement of extremely high ratio between the aqueous and organic phase was specified as semi-microextraction. A modified highly effective liquid phase semi-microextraction (LSME) procedure was developed for preconcentration and determination of ultra trace levels of inorganic antimony species in environmental waters using electrothermal atomic absorption spectrometry (ETAAS) for quantification. Antimony(III) species were selectively extracted as dithiocarbamate complexes from 100 mL aqueous phase into 250 μL xylene at pH range of 5–8. Total Sb was determined using the same extraction system over a sample acidity range of pH 0–1.2 without the need for pre-reduction of Sb(V) to Sb(III). The concentration of Sb(V) was obtained as the difference between that of total antimony and Sb(III). With an 8 min extraction an enrichment factor of 400 was achieved. The limit of detection (3 s) was 2 ng L −1 Sb. The method was not affected by the presence of up to 0.01% humic acid, 0.025 mol L −1 EDTA, 0.01 mol L −1 tartaric acid and 0.001 mol L −1  F − . Recoveries of spiked Sb(III) and Sb(V) in river, tap, and sea water samples ranged from 93 to 108%. The results for total antimony concentration in the river water reference material SLRS-5 were in good agreement with the information value. The procedure was applied to the determination and quantification of dissolved antimony species in natural waters.