氢化物发生原子荧光法直接测定锑及其化合物中的硒和铋

Direct Determination of Selenium and Bismuth in Antimony and Antimony Compound by Hydride Generation-Atomic Fluorescence Spectrometry

通过研究在不同酸度下Sb5+对Se ,Bi的干扰情况 ,发现在高酸度下 ,Sb对Se,Bi的干扰明显减弱 ,并结合锑在不同价态发生氢化反应的差异性 ,建立了不需通过任何化学分离而直接测定锑及其相关产品中的微量硒和铋的方法 ,并用于实际样品的分析。方法对实际样品加标回收率在 95 %～ 10 5 %之间 ,检测下限 (含量 )硒和铋分别为 0 0 0 0 0 4× 10 -2 mg·L-1和 0 0 0 0 1× 10 -2 mg·L-1,对实际样品分析精度分别为RSD(Se) =2 4 % (含量为 0 0 0 169× 10 -2 mg·L-1时 ) ,5 4 % (含量为 0 0 0 0 5 6× 10 -2 mg·L-1时 )和RSD(Bi) =5 0 % (含量为 0 0 0 0 2 4× 10 -2 mg·L-1时 ) ,1 3 % (含量为 0 0 0 2 2 9× 10 -2 mg·L-1时 ) ,完全满足实际样品分析的要求。

The interference of Sb in determination of Se and Bi in antimony powder and antimony compound has been studied in different acidity, It is found that the interference of antimony has been reduced apparently in high acidity. Simultaneously, according to the difference of hydride generation reaction between Sb5+ and Sb3+ a sensitive and rapid method has been developed and used to determine Se and Bi in real samples. The recovery of the method is 95%-105% for practical samples. Detection limits are 0.00004 x 10(-2)( content) for Se and 0.0001 x 10(-2) mg(.)L(-1) (content) for Bi respectively. The relative standard deviations of Se are 2.4% (content = 0.00169 x 10(-2) mg(.)L(-1)) and 5.4% (content = 0.00056 x 10(-2) mg(.)L(-1)). The relative standard deviations of Bi are 5.0% (content = 0.00024 x 10(-2) mg(.)L(-1)) and 1.3% (content = 0.00229 x 10(-2) mg(.)L(-1)) The method has been applied to determination of Se and Bi in practical samples with satisfactory results.