等离子质谱(ICP-MS)对高含量元素硫样品中的微量元素分析前处理方法初探  

Explore the method about pretreatment of analyzing trace element within high S-rich samples with Inductively Coupled Plasma Mass Spectrometry(ICP-MS)

作　　者：刘长华[1,2] 殷学博[1] 王晓媛[1,2] 袁春伟[1,2] 余少雄[1,2] 

机构地区：[1]中国科学院海洋研究所 [2]中国科学院研究生院,北京100039

出　　处：《海洋科学》2006年第9期1-5,共5页Marine Sciences

基　　金：国家自然科学基金项目项目(40376020);国家重点基础研究发展规划项目课题(G2000046701);中国科学院知识创新工程重要方向项目(KZCX3-SW-223);国家大洋重大专项课题(DY105-01-03-1)

摘　　要：用等离子质谱(ICP-MS)分析一些特殊样品的时候,前处理方法成为分析样品成功与否的关键,对于高基质含量的样品测量其微量元素含量更是如此。元素硫超过99%的自然硫样品中微量元素的测定一般使用燃烧的方法去除自然硫,但是一些易挥发性的元素也因此失去而测不出来。作者试图采用硫升华的方法去除硫基质,通过在原样品中加入内标,分析测定后计算内标的回收率确定出元素Be,Sn,Sc,U和稀土元素(REE)的回收率都在90%以上,可以用升华硫方法很好地测定,而元素Tl,Hf,W,Nb,Zr,Ta等的回收率则在75%以下,不适合用该种方法测定。Using Inductively Compled Plasma Mass Spectrometry（ICP-MS）,the pretreatment method of some special samples is a key, especially to analyzing trace elements of samples contained high background. Some native sulfur samples, which contain over 99% sulfur elements, generally are burned before analyzing trace elements with ICP-MS. But a amount of volatile-easy elements will not be decided. We try to wipe off background sulfur with sulfur-sublimation method, at the same time the standard-inner is added to the samples. After analyzing we calculate the callback ratio of most elements. Finally, the callback ratios are over 90% about elements Be, Sn, Sc, U and REE, so we may apply sulfur-sublimation method to pretreat high S-rich samples for analyzing trace element with ICP-MS. Otherwise the callback ratios are below 75% about elements T1, Hf, W, Nb, Zr, Ta, that is to say, sulfur-sublimation method is not applied to deciding these elements in high S-rich samples with ICP-MS.

关 键 词：等离子质谱(ICP-MS) 高基质 升华 回收率 

分 类 号：P59[天文地球—地球化学]