发展了一种硅胶负载纳米二氧化钛在线预富集矿石样品中的微量硒和碲并用氢化物发生-原子荧光光谱分析法检测的简单、灵敏且抗干扰能力强的分析方法。硒和碲被选择性吸附在微柱上,并可使用2%(m/v)NaOH洗脱。详细地研究了硒和碲的氢化物发生、吸附、解吸附条件和抗干扰情况。在优化的实验条件下,进样180s,硒和碲的检出限分别达到4.0和3.6ng·L^-1。灵敏度较传统的氢化物发生法分别提高了20和13倍。测定1μg·L^-1硒和碲的标准偏差(n=5)分别为0.7%和2.3%。该方法可用于测定矿石样品中的痕量硒和碲。
A simple,sensitive and interference-free method was established for simultaneous determination of trace selenium and tellurium in ore samples by HG-AFS,by using nano-TiO2 immobilized on a silica gel packed microcolumn for online preconcentration.Selenium and tellurium were selectively adsorbed to the microcolumn in acidic condition and then completely eluted with 2% (m/v)NaOH solution.The experimental conditions for hydride generation,adsorption,elution and potential interference were investigated in detail.Under the opti-mum conditions,the detection limits of selenium and tellurium by the proposed method with 180 s sampling time were 4.0 and 3.6 ng·L^-1 ,with sensitivity enhancement of 20-and 13-fold compared to conventional hy-dride generation method,respectively.The relative standard deviation (RSD,n=5)of this method for 1 μg· L^-1 Se(Ⅳ)and Te(Ⅳ)were 0.7% and 2.3%,respectively.This method was applied to determination of se-lenium and tellurium in several ore samples.