碲化镉溶液中无机痕量杂质成分分析标准物质研制  

Development of Reference Materials for the Analysis of Inorganic Trace Impurities in Cadmium Telluride Solutions

作　　者：张见营 崔彦杰[1] 周涛[1] 虞婧[2] 黄博崚 黎春 黄杏娇 刘芳美 朱赞芳 王金砖 肖光洋 王鑫磊 ZHANG Jian-ying;CUI Yan-jie;ZHOU Tao;YU Jing;HUANG Bo-ling;LI Chun;HUANG Xing-jiao;LIU Fang-mei;ZHU Zan-fang;WANG Jin-zhuan;XIAO Guang-yang;WANG Xin-lei(National Institute of Metrology,Beijing 100029,China;Shanghai Institute of Measurement and Testing Technology,Shanghai 201203,China;Chongqing Academy of Metrology and Quality Inspection,Chongqing 401121,China;State Nuclear Security Technology Center,Beijing 102445,China;Shenzhen Ningshen Inspection and Testing Technology Co.,Ltd,Shenzhen 518020,China;Zijin Copper Co.,Ltd,Longyan 364204,China;First Rare Materials Co.,Ltd,Qingyuan 511875,China;Nanjing Institute of Product Quality Inspection,Nanjing 210028,China)

机构地区：[1]中国计量科学研究院,北京100029 [2]上海市计量测试技术研究院,上海201203 [3]重庆市计量质量检测研究院,重庆401121 [4]国家核安保技术中心,北京102445 [5]深圳市宁深检验检测技术有限公司,广东深圳518020 [6]紫金铜业有限公司,福建龙岩364204 [7]广东先导稀材股份有限公司,广东清远511875 [8]南京市产品质量监督检验院,江苏南京210028

出　　处：《质谱学报》2022年第6期782-791,I0006,共11页Journal of Chinese Mass Spectrometry Society

基　　金：国家重点研发计划NQI重点专项(2019YFF0217101)。

摘　　要：本文研制了2 mg/g碲化镉(CdTe)溶液中无机痕量杂质成分分析的5种标准物质,每种包含21种杂质元素,浓度分别为0、1、2、4、8 ng/g。通过辉光放电质谱(GD-MS)法对CdTe原料纯度进行测量,筛选得到纯度>99.999%的高纯原料;使用HCl-HNO_(3)混酸将其溶解,再根据成分设计定量添加杂质元素,制备得到标准物质候选物。建立了基体匹配-内标校正-电感耦合等离子体质谱法用于标准物质定值与均匀性、稳定性检验,采用标准物质EB507验证方法可靠性。对包装容器溶出进行考察,以高密度聚乙烯(HDPE)作为包装容器可满足要求。采用建立的方法对全部元素进行检验,结果表明,标准物质均匀性以及长、短期稳定性良好,有效期12个月。通过8家实验室联合定值的方式,对标准物质中21种元素进行定值,以算数平均值作为标准值,并对不确定度进行全面、系统地评估。该系列基体标准物质填补了国内外空白,对于验证测量方法的可靠性、确保测量结果的一致性与溯源性具有重要作用。A series of matrix reference materials for 21 inorganic trace impurities in 2 mg/g cadmium telluride(CdTe)solution with five impurity concentration levels(0,1,2,4,8 ng/g)were developed.High purity(>99.999%)CdTe was used as raw materials and dissolved using HCl-HNO_(3) mixed acid,and then was doped with multi-elements solutions to prepare the candidate reference materials(RMs).Matrix-matched ICP-MS with internal standard calibration was established for certification,homogeneity test and stability test.Mass spectrum interferences of ^(106)Cd ^(1)H on ^(107)Ag and ^(114)In ^(1)H on ^(115)In could be effectively removed by optimizing argon gas flow parameters coupled with mathematical correction.The matrix suppressed effect was effectively corrected about 20%-60%by using matrix-matched method.The precision of consecutive analysis expressed as RSD(n=22)was reduced to approximately 1%by using internal standard calibration.The linearly correlation coefficient factors(R)of standard curves were greater than 0.999 for all elements.The limits of detection(LODs)ranged from 0.001 ng/g to 0.35 ng/g,and the spike recoveries ranged from 89.2%to 106.5%.The established method was further validated by using CRM EB507.The dissolution of packaging containers was investigated and the results showed that the impurity dissolution from HDPE(high density polyethylene)bottle was lower than that from PP(polypropylene)plastic bottle.Except for Ca and Se,the dissolution of elements of concern in 4 months was less than 0.2 ng/g,which met the requirement.All elements were tested by the established method,and the results showed that the homogeneity,long-term and short-term stability of RMs were satisfactory and the validity period was 12 months.The mass fractions of 21 elements were certified by using a collaborative characterization program with eight sophisticated participating laboratories and using HR-ICP-MS and Q-ICP-MS methods.The arithmetic mean values were taken as the certified values,and the uncertainty was systematically and comprehen

关 键 词：高纯碲化镉 杂质测量 标准物质 联合定值 基体效应 内标校正 电感耦合等离子体质谱(ICP-MS) 不确定度评估 

分 类 号：O657.63[理学—分析化学]