Lexa J, Stulík K
Chemical Laboratories, Central Research Institute, Skoda Works, Pilsen, Czechoslovakia.
Talanta. 1982 Dec;29(12):1089-95. doi: 10.1016/0039-9140(82)80223-3.
Arsenic, antimony and tin can be determined in the presence of one another by fast-scan differential-pulse polarography (FSDPP) on a single mercury drop in 1.5M hydrochloric acid. The reduction of As(III), Sb(III) and Sn(IV) to the metals is practically reversible and the reduction peaks are sufficiently separated. The lower limits of determination are 0.05, 0.005 and 0.001 mug/ml for As, Sb and Sn respectively, the calibration graphs exhibit very good linearity and the peak heights are reproducible. For application to alloy steels employed in nuclear technology, the elements to be determined must be separated from the matrix by extraction as their covalent bromides into toluene from concentrated sulphuric acid and back-extracted into the base electrolyte (1.5M HCl + 0.012M Br(-) + 0.03M hydrazinium sulphate). The recoveries of As, Sb and Sn are 100, 95 and 92% respectively and the relative error of determination is a few per cent.
在1.5M盐酸中，通过在单个汞滴上进行快速扫描差分脉冲极谱法（FSDPP），可以相互测定砷、锑和锡。As(III)、Sb(III)和Sn(IV)还原为金属的过程实际上是可逆的，且还原峰分得很开。As、Sb和Sn的测定下限分别为0.05、0.005和0.001μg/ml，校准曲线呈现出非常好的线性，且峰高具有重现性。对于应用于核技术的合金钢，必须通过将待测定元素以其共价溴化物的形式从浓硫酸中萃取到甲苯中，然后再反萃取到基础电解质（1.5M HCl + 0.012M Br(-) + 0.03M硫酸肼）中，从而与基体分离。As、Sb和Sn的回收率分别为100%、95%和92%，测定的相对误差为百分之几。
