锍镍试金富集-电感耦合等离子体质谱法测定铜阳极泥中微量元素铱铑  

Determination of Iridium and Rhodium in Copper Anode Slime by Inductively Coupled Plasma-Mass Spectrometry with Nickel Sulphide Fire Assay

作　　者：刘芳美 甘聪 廖彬玲 罗小兵 赖秋祥 LIU Fangmei;GAN Cong;LIAO Binling;LUO Xiaobing;LAI Qiuxiang(Zijin Copper Co.,Ltd.,Fujian Provine Key Laboratory for Green Production of Copper and Comprehensive Utilization of Associated Resources,Shanghang 364204,China)

机构地区：[1]紫金铜业有限公司,福建省铜绿色生产及伴生资源综合利用重点实验室,福建上杭364204

出　　处：《岩矿测试》2023年第2期298-306,共9页Rock and Mineral Analysis

基　　金：国家重点研发计划项目“国家质量基础的共性技术研究与应用”(2019YFF0217100)。

摘　　要：铜阳极泥富集了矿石、精矿或熔剂中绝大部分贵金属(如铱和铑),具有很高的综合回收价值。目前尚无铜阳极泥中铱和铑检测标准,而对其中铱和铑检测方法的开发是铱铑回收提取工作的重要前提。本文建立了锍镍试金富集结合电感耦合等离子体质谱法(ICP-MS)测定铜阳极泥中铱铑的检测技术。实验中通过锍镍试金捕集试样中的贵金属铱和铑,用50%盐酸溶解锍镍扣,使得含铱和铑的沉淀物与银及其他杂质元素有效分离,趁热过滤,铱铑沉淀物和滤膜转入封闭消解罐中以50%王水为介质溶解。试液采用ICP-MS直接测定铱和铑含量。实验优化了样品预处理条件,镍硫比为4∶1,时,熔渣为酸性,熔渣流动性和渣扣分离效果好且能有效捕集试样中铱和铑;锍镍扣溶解酸度为50%盐酸时,锍镍扣溶解反应合适且溶解完全,趁热过滤,其中银、镍、铜等杂质元素大部分被盐酸除去,达到了分离含铱和铑沉淀物与银及其他杂质元素的效果;密封消解温度和时间分别为160℃、2~3h时,铱和铑消解完全;选择合适的测定同位素可以消除可能存在的质谱干扰,以193 Ir和103 Rh为测定同位素、203 Tl和185 Re分别为铱和铑的内标时消除了信号漂移基体效应的影响。在优化的实验条件下测定铑和铱混合标准溶液系列,结果表明,铑和铱在10~100μg/L质量浓度范围内和铑及铱质谱强度与内标质谱强度之比呈线性关系,铱和铑的线性回归方程分别为y=36674.6 x+8264.7和y=45686.7 x+288.6,线性相关系数均大于0.999,方法检出限分别为0.007μg/L和0.011μg/L,定量下限分别为0.024μg/L和0.038μg/L。按照实验方法测定8个实际铜阳极泥试样中铱和铑,测定结果的相对标准偏差(RSD,n=7)为1.40%~4.57%,加标回收率为95.00%~103.65%。该方法能够满足铜阳极泥样品的检测要求。BACKGROUND:With the wide application of iridium and rhodium in aerospace,electronics,energy and other fields,it has become a very attractive metal in the world.In China,iridium and rhodium ore resources are relatively scarce with low grade,so it is essential to recover iridium and rhodium from secondary mineral resources.Copper anode slime enriches most of the precious metals such as iridium and rhodium in ores,which has high comprehensive recovery value.At present,there is no detection standard for iridium and rhodium in copper anode slime.The migration behavior of iridium and rhodium was not clear,so it was difficult to achieve directional enrichment and efficient extraction of iridium and rhodium metals.Therefore,the development of detection methods for iridium and rhodium in copper anode slime is an important prerequisite for the recovery and extraction of iridium and rhodium.OBJECTIVES:An analytical method for accurate determination of iridium and rhodium in copper anode slime was established to maximize the utilization of mineral resources and the recycling rate of iridium,rhodium and other precious metals.At the same time,it could provide data support for the purification of iridium and rhodium in copper anode slime.METHODS:In this paper,a method for determination of iridium and rhodium in copper anode slime by inductively coupled plasma-mass spectrometry(ICP-MS)with nickel sulphide fire assay was established.In the experiment,the precious metals iridium and rhodium in the sample were captured by nickel sulphide fire assay.The NiS beads were dissolved with 50%hydrochloric acid so that the precipitation of rhodium and iridium was separated from silver and other impurity elements through filtration when it was hot.The precipitates containing iridium and rhodium were effectively separated from silver and other impurity elements.The precipitate of iridium and rhodium with filter film were transferred into a closed digestion tank and dissolved in 50%aqua regia.The contents of iridium and rhodium in the solution

关 键 词：铱 铑 铜阳极泥 锍镍试金 电感耦合等离子体质谱法 

分 类 号：P641.12[天文地球—地质矿产勘探] P332.7[天文地球—地质学]