采用硝酸和盐酸低温加热溶解铜铟镓硒靶材样品,以将样品中的硒氧化为亚硒酸(H2SeO3),在水浴或低温下用尿素驱除硝酸,然后以盐酸为介质,采用亚硫酸将亚硒酸还原为单质硒沉淀,实现了硒与样品中其他元素的分离,将沉淀经抽滤烘干称重,通过计算得到靶材中硒含量,据此建立了重量法测定铜铟镓硒靶材中硒含量的方法.实验确立了测定的最佳条件,并进行了共存元素的干扰试验.结果表明,铜铟镓硒靶材中的铜、铟、镓对硒的测定无影响.采用实验方法测定铜铟镓硒靶材内控样品,测定值与理论配制值基本一致,相对标准偏差(RSD,n=11)在0.050%~0.48%之间.3家不同实验室结果平均值的最大误差不超过0.20%,相对标准偏差均小于0.50%.回收率试验表明硒的回收率在99%~101%之间.
The copper-indium-gallium-selenium target sample was dissolved with nitric acid and hydrochloric acid by low temperature heating.The selenium in sample was oxidized to seleninic acid (H2SeO3).The nitric acid was removed with urea in water bath or at low temperature.Then, the seleninic acid was reduced to elemental selenium precipitate using sulfurous acid in hydrochloric acid medium.The separation of selenium from other elements in sample was realized.The precipitate was filtered followed by drying and weighing.The content of selenium in target material could be obtained through calculation.Thus the determination method of selenium in copper-indium-gallium-selenium target by gravimetry was established.The optimum conditions for determination were established.Moreover, the interference tests of coexisting elements were conducted.The results showed that the copper, indium and gallium in target sample had no influence on the determination of selenium.The internal control sample of copper-indium-gallium-selenium target was determined according to the experimental method, and the found results were consistent with the theoretical values.The relative standard deviations (RSD, n=11) were between 0.050% and 0.48%.The maximum error of average determination result in three laboratories did not exceed 0.20%, and the RSD was less than 0.50%.The recovery test indicated that the recoveries of selenium were between 99% and 101%.
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