锡试金富集-电感耦合等离子体质谱法测定黑色页岩中的铂族元素  

ICP-MS Determination of Platinum Metals in Black Shale Enriched by Tin Fire Assay

作　　者：王君玉[1,2] 孙自军[1] 袁润蕾[1] 王盈[1] 李杰[1] 王敏捷[1] 

机构地区：[1]河南省岩石矿物测试中心,郑州450012 [2]国土资源部贵金属分析与勘查技术重点实验室,郑州450012

出　　处：《理化检验（化学分册）》2013年第8期972-975,978,共5页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：国土资源部公益性行业专项(200911043-01)

摘　　要：黑色页岩中的铂族元素经锡试金富集后，所得贵金属沉淀物用盐酸-硝酸（3＋1）混合酸溶解，用电感耦合等离子体质谱法测定样品中的铂族元素。以镥为内标元素，用轻质氧化镁-高纯碳化硅（2＋1）作覆盖剂，以防止锇和钌的挥发损失。铂族元素在一定的质量浓度范围内与其光谱强度呈线性关系，检出限（3a）在0．018-0．20ng·g叫之间。方法的加标回收率在80．0％～110％之间，相对标准偏差（n=11）a-5．9％～14％之间。Platinum metals in black shale were enriched hy the method of tin fire assay. The precious metal precipitate obtained was dissolved in mixed acid of HC1-HNOa （3 ＋ 1）, and contents of platinum metals in the solution were determined by ICP-MS. Lutetium was used as internal standard; and a mixture of light MgO and high purity SiC （2＋1） was used as covering reagent to avoid the volatilization of Os and Ru. I.inear relationships between values of spectral intensity and mass concentration of the platinum metals were kept in definite ranges. Detection limits （30） found were in the range of 0. 018--0. 20 ng g-1. Tests for recovery were made by standard addition method, giving values of recovery in the range of 80. 0%--110 with RSD＇s （= 11） in the range of 5.9-140A.

关 键 词：电感耦合等离子体质谱法 铂族元素 锡试金 黑色页岩 

分 类 号：O657.63[理学—分析化学]