D_(290)树脂-活性炭吸附富集电感耦合等离子体质谱法测定铜精矿中铂钯  

Determination of Pt and Pd in Copper Concentrate Ores by ICP-MS Using D_(290) Anion Exchange Resin and Activated Charcoal for Concentration

作　　者：胡德新[1] 谷松海[1] 任海 马德起[1] 杨丽飞[1] 苏明跃[1] 

机构地区：[1]天津出入境检验检疫局化矿金属材料检测中心,天津300456 [2]天津口岸检测分析开发服务有限公司,天津300457

出　　处：《岩矿测试》2013年第4期572-575,共4页Rock and Mineral Analysis

基　　金：天津市滨海新区塘沽科技发展专项资金项目(2012STHB04-04)

摘　　要：矿产品中痕量贵金属元素的测定通常需要富集分离,在检测过程中谱线干扰较多。本文对铜精矿样品在高温下灼烧除去碳和硫,采用盐酸+王水+氢氟酸消解体系进行分解,利用D290阴离子交换树脂-活性炭作为吸附剂富集铂和钯,以Y、In、Bi为内标元素,105Pd和195Pt作为测量同位素,用电感耦合等离子体质谱法(ICP-MS)测定铂和钯的含量。铂和钯的吸附率均达到90%以上,加标回收率分别为92.0%和96.0%,检出限分别为0.126 ng/g和0.105 ng/g,方法精密度(RSD,n=6)小于4%。应用于实际铜精矿样品分析,测定值与锍镍试金-ICP-MS测定结果一致。本法的样品处理体系最大限度地减少了样品中其他金属离子对待测元素的影响,选择的内标元素和高纯氦碰撞反应可有效地减少基体效应和同质异位素干扰。相比于锍镍试金法,该方法的样品前处理简单,铂和钯的富集效果明显,测定检出限低。Determination of trace elements in minerals usually requires pre-concentration and separation with many spectral line interferences during measurement. The concentrate ores were calcined at high temperature to remove the C and S. The calcinates were then digested by using the HCl-auqa regia-HF acids system. The D290 anion exchange resin and activated charcoal procedures were conducted to enrich Pt and Pd. The contents of Pt and pd were obtained by Inductively Coupled Plasma-Mass Spectrometry （ICP-MS） with internal standard elements of Y, In and Bi and measured isotopes of 105Pd and 195Pt. The absorption property and separation conditions of D290 anion exchange resin to trace Pt and Pd in copper concentrate ores were studied. The enrichment effects of Pt and Pd were above 90%, the recoveries were 92.0% and 96.0%, and the relative standard deviations （RSD, n=6） were smaller than 4%. The detection limits of the method were 0.126 ng/g and 0.105 ng/g for Pt and Pd. The presented method mostly reduced the inferences from other ions to the target elements of Pt and Pd. Moreover, the collision reaction between the internal standard elements and high purity Ar effectively reduced the matrix effect and isobaric interference. Five random geological samples were analyzed by this method in comparison with the method of NiS fire assay ICP-MS and the established method had the advantages of simple pretreatment and high enrichment of Pt and Pd with lower detection limits.

关 键 词：铜精矿 铂 钯 D290阴离子交换树脂 活性炭 电感耦合等离子体质谱法 

分 类 号：O614.121[理学—无机化学] O614.826[理学—化学]