预还原氢化物发生-原子荧光光谱法快速测定化探样品中的As、Sb、Bi、Hg  

Quick Determination of As,Sb,Bi,Hg in Geochemical Samples by Prereduction Hydride Generation-Atomic Fluorescence Spectrometry

作　　者：罗治定[1] 陈庆芝[1] 金倩[1] 李晓敬[1] 孙孟华 李丹 LUO Zhiding;CHEN Qingzhi;JIN Qian;LI Xiaojing;SUN Menghua;LI Dan(Hebei Central Laboratory of Geology and Mineral Resources,Baoding,Hebei 071051,China)

机构地区：[1]河北省地矿中心实验室,河北保定071051

出　　处：《中国无机分析化学》2018年第2期17-21,共5页Chinese Journal of Inorganic Analytical Chemistry

摘　　要：通过对化探样品进行王水密闭溶解,饱和的硫脲-抗坏血酸预还原,运用氢化物发生-原子荧光光谱法实现了地质样品中As、Sb、Bi、Hg元素的任意配对以及连续快速测定。实验确定了原子化器高度为14mm,最佳溶样时间为1h。在优化条件下,结果显示还原剂(硫脲-抗坏血酸)对Hg、Bi测定结果无影响,且Hg、Bi测定结果在预还原20min至48h内都很稳定,测定结果良好,Cu、Co、Ni、Au、Ag、Cd、As、Sb、Bi、Se、Ge等金属离子对预还原测定汞均无干扰,对比实验表明还原剂体系下汞荧光强度值基本不变。方法的检出限低、精密度好、准确度高、操作简便,有效避免了元素污染问题,可满足大批量地质样品分析测定的需要。The arbitrary matching and continuous rapid determination of As,Sb,Bi,Hg in geochemical samples were achieved through hydride generation-atomic fluorescence spectrometry.The samples were dissolved in sealed vessels with aqua regia and prereduced by saturated thiourea-ascorbic acid.The results showed that the optimum atomizer height was 14 mm with 1 hour sample dissolution time.Under the optimized conditions,the reducing agent(thiourea-ascorbic acid)had no effect on the determination of Hg and Bi,showing stable and excellent results for the prereduction time from 20 minutes to 48 hours.Comparative experiment showed that in the reductant system,the fluorescence intensity of Hg showed no substantial change or interference with the Cu,Co,Ni,Au,Ag,Cd,As,Sb,Bi,Se,Ge and other metal ions.This method has low detection limit,high precision and accuracy,simple operation,can effectively avoiding the problem of elemental pollution and is suitable for the analysis of multitudinous geochemical samples.

关 键 词：预还原 原子荧光光谱法 地质样品 砷 锑 铋 汞 

分 类 号：O657.31[理学—分析化学] TH744.16[理学—化学]