巯基葡聚糖凝胶分离富集—氢化物发生原子荧光法测定地球化学样品中锑  

Determination of antimony in geochemical samples by hydride generation-atomic fluorescence spectrometry after separation and enrichment with mercapto-dextrangel

作　　者：张锂[1] 韩国才[1] 

机构地区：[1]兰州工业高等专科学校基础学科部

出　　处：《冶金分析》2007年第6期24-27,共4页Metallurgical Analysis

基　　金：甘肃省教育厅资助项目(0612-03)

摘　　要：建立了采用巯基葡聚糖凝胶分离富集,氢化物发生原子荧光法测定地球化学样品中锑的方法。以微波消解分解样品,缩短了样品处理时间,避免了挥发组分的损失。经巯基葡聚糖凝胶吸附柱分离富集锑,用6.0 mol/L HCl洗脱,氢化物发生原子荧光法测定。通过试验确定了仪器最佳工作条件,吸附和洗脱条件,氢化物发生最佳条件及微波消解程序,并对共存干扰元素的允许量进行了研究。在此条件下测定锑,得出该方法的检出限为0.25μg/L,线性范围0.001～0.20 mg/L,相对标准偏差(n=6)为2.9%～5.1%,加标回收率99.2%～104.5%。方法应用于国家一级地球化学标准物质中锑的测定,结果与认定值基本相符。A method for the determination of antimony in geochemical samples by hydride generation-atomic fluorescence spectrometry after separation and enrichment with mercapto-dextrangel was developed. By using micro-wave assisted digestion procedure with hydrofluoric acid, hydrochloric acid and nitric acid to dissolved sample, The decrease in the time of preparing sample was achlved and loss of volatile components could be avoided. The sample solution was allowed to pass through adsorbing column with mercapto-dextrangel at pH 2, then antimony adsorbed on the column was eluted with 6. 0 mol/L hydrochloric acid. Working conditions of atomic fluorescence spectrometer, conditions for hydride generation of antimory and microwave digestion were optimized. Meanwhile allowable amounts of interfering element was studied in the determination of antimony. The liner range of the method is 0. 001-0. 20 mg/L for antimony. The detection limit of the method was 0. 25 μg/L The method has been applied to the determination of antimony in national geochemical certified reference materials and the results obtained are in good agreement with certified values,giving the RSD of 2. 9%-5. 1% （n=6）and the recovery of 99. 2%-104. 5%.

关 键 词：巯基葡聚糖凝胶 分离富集 氢化物发生 原子荧光法 锑 

分 类 号：O657.31[理学—分析化学]