等离子质谱(ICP-MS)对高含量元素硫样品中微量元素分析的前处理方法比较

Comparing burning and sublimation methods in pretreatment of high element sulfur samples for microelement analysis with Inductively Coupled Plasma Mass Spectrometry (ICP-MS)

如何去除元素硫高含量样品的背景硫，是测定该类样品中微量元素成功的关键．通过分别对样品进行燃烧和升华两种前处理方法的研究对比，得出用升华的方法处理自然硫样品对于其微量元素的测定可靠性大，所测定微量元素回收率的优良率是68％，燃烧法处理后测定微量元素回收率的优良率是64％．而且前者优良回收率的范围是79．9％～120．5％，明显高于后者的优良回收率范围76．2％～98。0％．对于这样的结果，温度是主要的控制因素．燃烧法处理样品温度条件较难控制，升华法则可以较严格的控制温度，从而减少被测元素的散失，能得到较为理想的数据．

How to wipe off sulfur-background is a key step to quantify microelements in certain samples containing high concentration of sulfur. By comparing data from both burning and sublimation methods for pretreatment samples containing high sulfur, it suggested that the sublimation method gave a much reliable result. The choiceness ratio of recovery is 68% for decided microelements by sublimation method, while the choiceness ratio of recovery is 64% by burning method. Moreover, the former range of recovery is 79.9% ～ 120.5% which is higher than the latter, ranging the recovery from 76.2% to 98.0%. The temperature is the key factor to be controlled, as its significant influence to the results. It is difficult to control the burning method and it is easy for sublimation method. Thereby better data can be achieved by decreasing element-decided loss with sublimation method of pretreatment.