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Abstract
The methodology for antimony speciation was optimized for liquid chromatography coupled to hydride generation – atomic fluorescence spectrometry. An anion exchange column was employed with isocratic elution. Ammonium tartrate was shown to be the optimum mobile phase and extracting solution for this analysis. The highest efficiency and resolution for the antimony species was achieved using 5 percent methanol in 300 millimoles per liter ammonium tartrate acidified with hydrochloric acid to pH 4.5. The retention times of antimony(V), trimethylantimony, and antimony(III) were 2.6, 3.9, and 5.2 minutes, respectively. The calibration curves were linear with limits of detection of 0.1, 0.2, and 0.43 microgram per liter for antimony(III), antimony(V), and trimethylantimony, respectively. The precision, evaluated by the relative standard deviation, ranged from 1.2 to 5.3 percent. The average recovery from these environmental samples by a single-step procedure was approximately 26 percent. The results also revealed that the correlation between the sum of each species by the single-step procedure and total digestion was significant for the investigated soils and sediments.