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微量硒的测定多采用3,3’—二氨基联苯胺比色法,由于该试剂对人有害已不生产,我们试验了于6.5—10N盐酸中以三氯甲烷萃取Se~(4+)与甲乙酮生成的(RCOCHR)_2SeCl_2络合物,使其与大量的Cu~(2+)、Pb~(2+)、Zn~(2+)、Cd~(2+)、Co~(2+)、Ni~(2+)、Bi~(3+)、Fe~(3+)、Te~(4+)等分离。有机相经处理后于12%亚硫酸钠—8%碳酸钠底液中进行硒的示波极谱测定,峰电位于-0.39伏。本法灵敏度高,重现性好,可侧定范围0.0X—0.0000X%. 测定:试样经硝酸溶解,高氯酸冒烟,
The determination of trace selenium use 3,3’-diaminobenzidine colorimetric method, as the reagent is not harmful to human production, we tested in 6.5-10N hydrochloric acid with chloroform extraction of Se ~ (4 +) and Methyl ethyl ketone (RCOCHR) _2SeCl_2 complex, with a large number of Cu 2 +, Pb 2 +, Zn 2 +, Cd 2 +, Co 2+ , Ni ~ (2 +), Bi ~ (3 +), Fe ~ (3 +), Te ~ (4 +) and so on. The oscillopolarographic determination of selenium in the organic phase was performed on 12% sodium sulfite-8% sodium carbonate bottom solution with peak potential at -0.39 volts. This method has high sensitivity, good reproducibility, can be scaled range 0.0X-0.0000X%. Determination: The sample was dissolved by nitric acid, perchloric acid smoke,