电感耦合等离子体原子发射光谱法测定核纯级海绵锆中17种微量杂质元素  

ICP-AES Determination of 17Kinds of Trace Impurity Elements in Sponge Zirconium of Nuclear Purity Grade

作　　者：李洁[1] 安身平[1] 宁伟 秦毅[1] 

机构地区：[1]中国核动力研究设计院反应堆燃料及材料国家重点试验室,成都610213

出　　处：《理化检验（化学分册）》2017年第9期1047-1051,共5页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

摘　　要：向2.500 0g样品中加入3mol·L^(-1)硝酸溶液10mL后滴加氢氟酸至溶解完全,冷却后定容至50mL。取此样品溶液5.00mL,加入若干17种元素的混合标准溶液并由3mol·L^(-1)硝酸溶液定容至50mL,采用电感耦合等离子体原子发射光谱法测定各元素的含量。标准加入法可克服基体干扰,各元素分析线的强度与其质量浓度呈线性关系。Co、Cu、Mn、Mo、Ni、Pb、V、Ti的线性范围为0.10~2.0mg·L^(-1),Al、Cr、Hf、Mg、Nb、Ta、Zn的线性范围为0.20~4.0mg·L^(-1),Fe、Sn的线性范围为0.40~8.0mg·L^(-1),17种微量杂质元素的检出限(3s)在1.0~50μg·L^(-1)之间。加标回收率在90.0%~108%之间,测定值的相对标准偏差(n=6)小于10%。The sample （2.500 0g） was dissolved in 10 mL of 3 mol·L^-1 nitric acid solution with dropwise addition of hydrofluoric acid.After cooling and making up its volume to 50 mL,5.00 mL of the sample solution was mixed with definite amount of mixed standard soluntion of the 17 kinds of elments,and diluted with 3 mol·L^-1nitric acid solution to 50 mL for ICP-AES detemination of the 17 kinds of elements.Matrix interference was effectively overcomed by using standard addition method.Linear relationships were found between the intensity of anlaytical lines and the mass concentrations of the 17 kinds of elements.The linearity range of Co,Cu,Mn,Mo,Ni,Pb,V and Ti was 0.10-2.0mg·L^-1,the linearity range of Al,Cr,Hf,Mg,Nb,Ta and Zn was 0.20-4.0mg·L^-1,and the linearity range of Fe and Sn was 0.40-8.0mg·L^-1.Detection limits （3s） of 17 kinds of elements were in the range of 1.0-50μg·L^-1.Recovery rates obtained by standard addition method ranged from 90.0% to 108%,and RSDs （n=6） were less than 10%.

关 键 词：电感耦合等离子体原子发射光谱法 微量元素 核纯级海绵锆 标准加入法 

分 类 号：O657.31[理学—分析化学]