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利用硒元素的易挥发性,研制了一个用于微量硒样品的蒸发提纯装置,用所建立提纯流程纯化了购买的76Se、78Se和82Se3个浓缩同位素试剂。对比样品分离前后的电感耦合等离子体质谱(ICP-MS)半定量方法测定结果,该方法能够有效地将钠、钾、铁和钨等为主的干扰元素去除,纯化后样品中硒的纯度可以达到99.99%以上,样品回收率约为90%。经多接收电感耦合等离子体质谱(MC-ICP-MS)分析样品纯化前后的硒同位素丰度,整个纯化过程没有改变硒的同位素组成。
Based on the volatility of selenium, an evaporation and purification device for trace selenium samples was developed. The purchased 76Se, 78Se and 82Se3 concentrated isotopes were purified by the established purification procedure. The results of semi-quantitative analysis by inductively coupled plasma mass spectrometry (ICP-MS) before and after the separation of samples show that the method can effectively remove the interfering elements such as sodium, potassium, iron and tungsten, and the purity of the purified selenium can be Reached 99.99%, the sample recovery rate was about 90%. The abundances of selenium isotopes before and after purification were analyzed by multi-inductively coupled plasma mass spectrometry (MC-ICP-MS), and the isotopic composition of selenium was not changed during the whole purification.