Trivalent antimony was determined in acid medium(pH3.6) under the
optimized condition (deposition potential of−0.7V, deposition time of 180s, ionic strength of 0.3M and oxidant mercury concentration of 10mg l−1). Total antimony was determined after quantitative reduction of Sb(V)withl-cysteine (1.5%,w/v) and its concentration was calculated from sifferencebetween the total antimony and Sb(III). The developed method provided two distinct linear calibration one ranging from 10
up to 50?gl−1 and other from 100 up to 800?gl−1 with respective correlation coefficient of 0.9978 and 0.9993, presenting detection limit of 6.2?gl−1 . Repeatability for the six independent samples expressed in terms of relative standard deviation was found to be 3.01 and 1.39% for 40.0 and 300.0?gl−1 antimony concentration, respectively. Results on the effect of foreign substances [Al(III), Mg(II), Fe(III), Cd(II), Zn(II) and meglumine] on analytical signal of antimony showed no interference even using high content of foreign ions in the analyte:interferent ratio up to 1:100. The proposed method was successfully applied for the speciation of Sb(III) and Sb(V) in pharmaceutical formulation and the accuracy was assessed from addition and recovery tests as well as comparing with graphite furnace atomic absorption spectrometry (GF AAS) technique used as reference analytical method.
Trivalent antimony was determined in acid medium(pH3.6) under theoptimized condition (deposition potential of−0.7V, deposition time of 180s, ionic strength of 0.3M and oxidant mercury concentration of 10mg l−1). Total antimony was determined after quantitative reduction of Sb(V)withl-cysteine (1.5%,w/v) and its concentration was calculated from sifferencebetween the total antimony and Sb(III). The developed method provided two distinct linear calibration one ranging from 10up to 50?gl−1 and other from 100 up to 800?gl−1 with respective correlation coefficient of 0.9978 and 0.9993, presenting detection limit of 6.2?gl−1 . Repeatability for the six independent samples expressed in terms of relative standard deviation was found to be 3.01 and 1.39% for 40.0 and 300.0?gl−1 antimony concentration, respectively. Results on the effect of foreign substances [Al(III), Mg(II), Fe(III), Cd(II), Zn(II) and meglumine] on analytical signal of antimony showed no interference even using high content of foreign ions in the analyte:interferent ratio up to 1:100. The proposed method was successfully applied for the speciation of Sb(III) and Sb(V) in pharmaceutical formulation and the accuracy was assessed from addition and recovery tests as well as comparing with graphite furnace atomic absorption spectrometry (GF AAS) technique used as reference analytical method.
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