小试金-碲保护留铅灰吹富集测定矿石中痕量贵金属  

Determination of Trace Precious Metals in Ores by Te Protection and Cupellation Retain Lead-Minified Fire Assay

作　　者：邵坤[1] 范建雄[1] 李可及[1] SHAO Kun;FAN Jianxiong;LI Keji(Institute of Multipurpose Utilization of Mineral Resources,Chinese Academy of Geological Science,Chengdu 610041,China)

机构地区：[1]中国地质科学院矿产综合利用研究所

出　　处：《贵金属》2019年第3期66-69,83,共5页Precious Metals

基　　金：中国地质调查局地质调查项目(DD20189507)

摘　　要：采用小铅试金富集,以5 mg碲为灰吹保护剂,通过留铅灰吹法将矿石样品中痕量贵金属(金、铂、钯、铑、铱和钌)定量富集在50 mg左右的铅合粒中。铅合粒先以(1+1)硝酸溶解,再加入盐酸进一步增强溶解能力,基体通过以氯化铅形式沉淀得以分离,采用电感耦合等离子体质谱法(ICP-MS)测定。相对标准偏差(RSD,n=6)为:Au 4.6%、Pt 8.7%、Pd 4.5%、Rh 9.2%、Ir 6.1%、Ru 5.8%。方法用于国家一级标准物质和黑色页岩样品中痕量贵金属的测定,测定值与认定值基本吻合。The trace precious metals in ores were collected by minified lead fire assay using 5mg Te as protective agent and cupellation retain lead of about 50 mg.The lead alloy was first dissolved in(1+1)HNO3,and then added HCl to form aqua regia to enhance dissolution capability.The lead matrix was separated as PbCl2 precipitate to eliminate interference in the following ICP-MS measurements.The relative standard deviations(n=6)of national standard materials were 4.6%,8.7%,4.5%,9.2%,6.1%and 5.8%for Au,Pt,Pd,Rh,Ir and Ru,respectively.The determination results of national standard materials and black shale samples were consistent with the recommended value.

关 键 词：分析化学 小铅试金 碲保护剂 留铅灰吹 电感耦合等离子体质谱(ICP-MS) 贵金属 

分 类 号：O657.63[理学—分析化学]