焙烧分离-氢化物发生-原子荧光光谱法测定土壤样品中微量硒

采用艾斯卡试剂(碳酸钠和氧化锌)作焙烧试剂,半熔法分解样品,沸水提取,分离出Cu、Co、Ni等过渡金属元素,氢化物发生-原子荧光光谱法测定土壤样品中微量硒。通过正交试验确定了测定方法的仪器和试剂条件,考察了Cu、Ni、Fe、Al、Pb、Au、As、Bi、Sb、Pt等共存元素的干扰情况。方法检出限为0.0135μg/g,回收率为87.0%~123.0%。对多个土壤国家一级标准物质进行测定,其结果与标准值相符。方法同时适合于地质样品及多金属矿中硒的测定。

Determination of Trace Selenium in Soil Samples by Hydride Generation-Atomic Fluorescence Spectrometry with Baking Separation

A method for the determination of trace selenium in soil samples by hydride generation-atomic fluorescence spectrometry with baking separation was proposed in this paper.Samples were semi-melted by baking with Na2CO3 and ZnO mixture as a baking agent and the melt was then dissolved with boiling water,the transition elements including Cu,Co,Ni,etc.were separated.Trace selenium in the soil sample solution was then determined by hydride generation-atomic fluorescence spectrometry.The operation conditions for the determination were optimized by the orthogonal experiments.The interferences from the coexistent elements of Cu,Ni,Fe,Al,Pb,Au,As,Bi,Sb and Pt on the selenium determination were studied.The detection limit of the method for selenium is 0.0135 μg/g and the recovery is 87.0%~123.0%.The method has been applied to the determination of trace selenium in National Standard Reference Materials and the results are in agreement with certified values.