高基体样品进样系统-电感耦合等离子体质谱法测定进口铜精矿中稀土元素的含量  

Determination of Rare Earth Elements in Imported Copper Concentrate by Inductively Coupled Plasma Mass Spectrometry With High Matrix Injection System

作　　者：王斌[1,2] 郑少锋 李伟才 钟康华 甘久林 杨中民[1] 宋武元[3] WANG Bin;ZHENG Shao-feng;LI Wei-cai;ZHONG Kang-hua;GAN Jiu-lin;YANG Zhong-min;SONG Wu-yuan(State Key Laboratory of Luminescent Materials and Devices,South China University of Technology,Guangzhou 510641,China;State Key Testing Laboratory of Consumer Products,Huangpu Customs Technology Center,Dongguan 523070,China;Guangzhou Customs District Technology Center,Guangzhou 510623,China)

机构地区：[1]发光材料与器件国家重点实验室,华南理工大学,广东广州510641 [2]国家消费品安全检测重点实验室,黄埔海关技术中心,广东东莞523070 [3]广州海关技术中心,广东广州510623

出　　处：《光谱学与光谱分析》2022年第6期1822-1826,共5页Spectroscopy and Spectral Analysis

基　　金：国家重点计划研发项目(2018YFF0215400)资助。

摘　　要：铜精矿的铜含量在20%~30%,是冶炼铜的基础矿物原料,由于地质因素和冶炼技术的差别,世界各矿区铜精矿的等级存在差异,加之近年来,铜精矿掺假造假、伪报瞒报、有毒有害元素超标等案件多发,对国家和人民的生活和经济发展造成了危害,建立进口铜精矿产地溯源和特征成分分析方法,在口岸执法方面可以提供有效技术支持。本研究应用电感耦合等离子体质谱仪测定铜精矿样品中的钇、镧、铈、镨、钕、钐、铕、钆、铽、镝、钬、铒、铥、镱、镥等15种稀土元素含量。铜精矿的物理化学性质相对稳定,针对铜精矿中稀土元素的消解方法有碱熔法、微波消解酸溶法和常压酸溶法,实验采用改进的常压酸溶法对样品进行消解,选取具有代表性的5^(#),6^(#),13^(#),16^(#)和18^(#)不同稀土元素含量的铜精矿样品,通过对氢氟酸、高氯酸、勒福特王水三种强酸的加入顺序和用量进行试验,得到了所有铜精矿样品能够完全溶解,而且用量合理的混合强酸体系最佳方案为3 mL氢氟酸-1 mL高氯酸-3 mL勒福特王水。铜精矿属于高基体样品,其硅酸盐、碳酸盐等高盐化合物会对稀土元素分析带来基体干扰,本研究比较了电感耦合等离子体质谱仪的普通模式和高基体样品进样模式下样品的分析效果,普通模式时稀土元素工作曲线的一元线性结果较差,高基体进样模式时工作曲线的线性相关系数都在0.9994以上,定量范围在2.25~110.00 mg·kg^(-1),检出限在0.0081~0.0725μg·L^(-1)。选取13^(#)铜精矿样品进行方法的回收率试验,回收率在97.4%~103.0%,精密度小于3.1%。同时,选用与铜精矿样品组成相似的GBW07105玄武岩岩石成分分析标准物质和GBW07234铜矿石标准物质,按照本实验方法,对稀土元素含量进行测定,考察了在本方法测定范围内的稀土元素Y,La,Ce,Pr,Nd,Sm,Gd和Dy的含量,测定值都在标准物质标准值范围内。该�Copper concentrate has a copper content of 20%~30%,which is the basic mineral raw material for copper smelting.Due to the difference between geological factors and smelting technology,the grade of copper concentrate in various mining areas in the world is different.In recent years,copper concentrate adulteration,false report and concealment,toxic and harmful elements exceeding the standard cases frequently occur,causing harm to the country and people’s life and economy.Establishing the origin traceability and characteristic component analysis method of imported copper concentrate can provide effective technical support to port law enforcement.The contents of 15 rare earth elements,such as yttrium,lanthanum,cerium,praseodymium,neodymium,samarium,europium,gadolinium,terbium,dysprosium,holmium,erbium,thulium,ytterbium and lutetium,in copper concentrate samples were determined by inductively coupled plasma mass spectrometry.The chemical and physical properties of copper concentrate is relatively stable,aiming at the digestion method of rare earth elements in copper concentrate with acid-soluble alkali fusion method,microwave method and the method of atmospheric acid-soluble.This experiment adopts the samples improved atmospheric acid-soluble method to eliminate and select a representative sample of 5^(#),6^(#),13^(#),16^(#),18^(#)samples of different rare earth elements content of copper concentrate,Through the tests on the addition order and dosage of hydrofluoric acid,perchloric acid and Lefter aqua regia,the best solution of the mixed strong acid system with reasonable dosage was 3 mL hydrofluoric acid-1 mL perchloric acid-3 mL Lefter aqua regia,which could completely dissolve all copper concentrate samples.Copper concentrate was a high substrate samples that silicate and carbonate salt compounds can bring matrix interference analysis of rare earth elements.In this study,the analysis results of the common mode of ICP-MS and the high matrix sample injection mode were compared.The unary linear results of rare eart

关 键 词：铜精矿 电感耦合等离子体质谱仪 稀土 

分 类 号：O657.31[理学—分析化学]