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锑是钢中有害元素,含量一般小于0.01％。萃取比色要预先分离Fe~(3+),操作繁复。近年来出现了氢化物——原子荧光光谱法,阳极溶出伏安法的测定方法。目前报导的三苯甲烷染料和罗丹明C与SbCl_6~-形成缔合物的阴极伏安法,选择性、灵敏度及操作上均不够理想。作者发现噻嗪染料与锑的络阴离子缔合物进行阴极伏安法测定时,具有较好的选择性和灵敏度,尤以新亚甲蓝(New methylene blue简称NMB)最佳。为此作了底液条件和电化学条件试验,干扰离子试验和在大量高铁存在下锑(Ⅴ)的定量还原试验。拟定了阴极伏安法直接测定钢中痕量锑的方法,检测下限可达到5×10~(-6)％。
Antimony is harmful elements in steel, the content is generally less than 0.01%. Extraction of color to be separated in advance Fe ~ (3 +), complicated operation. In recent years, hydride generation - atomic fluorescence spectrometry, anodic stripping voltammetry method. The currently reported cathodic voltammetric methods for the formation of association of triphenylmethane dyes with rhodamine C and SbCl 6 ~ - are not ideal for their selectivity, sensitivity and operation. The authors found that the complex of thiazine dye and antimony complex anion cathodic voltammetry has good selectivity and sensitivity, especially the best of new methylene blue (NMB). For this reason, the bottom liquid condition and electrochemical conditions test, interference ion test and quantitative reduction test of antimony (Ⅴ) in the presence of a large amount of high-speed rail were made. The direct voltammetry method for the determination of trace antimony in steel was developed. The detection limit can reach 5 × 10 -6%.