锑的野外快速分析方法——氢化物发生-光导分光光度法

Rapid Field Method for Antimony Analysis--Determination of Antimony by Hydride Generation-Fibre-Optic Spectrophotometry

详细考察了用氢化物发生-光导比色法在野外实验条件下测定Sb的各种条件及影响因素,制定了适合野外的氢化物发生-光导比色快速测定锑的方法。样品经王水封闭溶解后, 在掩蔽剂存在下,用自制的硼氢化钾片使经预还原的Sb生成氢化物逸出,将吸收液中的Fe(Ⅲ) 还原为Fe(Ⅱ)与邻菲哆啉显色,用自行开发、研制的光导分光光度(比色)计进行比色测定。方法的检出限(3s)为0．18μg/g,加标回收率为96．0％-98．0％,11次测定的精密度(RSD)小于 8．2％。方法经国家一级标准物质验证,分析结果与标准值吻合。

A rapid field method for determination of antimony by hydride generation-fibre-optic spectrophotometry was developed and some factors affecting the antimony analysis were studied. The sample is digested with aqua regia and the mixed masking reagents are added into the sample solution to eliminate the interference from coexistant elements. The hydride of antimony reduces Fe （ Ⅲ ） to Fe （ Ⅱ ）. Fe （ Ⅱ ） and 1,10-phenantholine formed red complex in pH≈3. Maximum absorbtive wavelength of the red complex is 510 nm. The detect limit of the method is 0.18 μg/g for antimony. The method has been applied to the determination of trace antimony in national standard reference samples and the results are in agreement with certified values with precision of less than 8.2% RSD（n = 11 ）. The recoveries of standard addition are 96.0% -98.0%.