电感耦合等离子体原子发射光谱法测定核级锆合金中铁、镍、铌、锡  

Determination of Fe,Ni,Nb and Sn in nuclear-grade zirconium alloys by ICP-AES

作　　者：郭国龙[1] 王春叶[1] 杜凯华 龚明明[1] 曹淑琴[1] 黄辉[2] 刘霞[2] GUO Guolong;WANG Chunye;DU Kaihua;GONG Mingming;CAO Shuqin;HUANG Hui;LIU Xia(Beijing Research Institute of Chemical Engineering and Metallurgy,Beijing 101149,China;Institute 53,China North Industries Group Corporation,Jinan 250031,China)

机构地区：[1]核工业北京化工冶金研究院,北京101149 [2]中国兵器工业集团第五三研究所,济南250031

出　　处：《化学分析计量》2022年第12期51-54,共4页Chemical Analysis And Meterage

基　　金：国防科工局技术基础项目(JSJL2019208A008)。

摘　　要：采用基体匹配法,建立了电感耦合等离子体原子发射光谱测定锆合金中铁、镍、铌、锡4种常量元素的分析方法。通过用高纯海绵锆进行基体匹配和样品最佳溶解试验,准确测定了核级锆合金中常量元素铁、镍、铌、锡,两个元素含量不同样品的加标回收率分别为98.5%~99.5%和102%~104%,相对标准偏差均小于2%(n=10),满足西屋认证标准要求。铁、镍质量浓度在0~10 mg/L,铌、锡质量浓度在0~100 mg/L内线性良好,相关系数均为0.999 9。铁、镍、铌、锡的检出限分别为2.29、1.21、1.83、58.7μg/g,测量下限分别为7.62、4.04、6.11、196μg/g。A method for determining Fe, Ni, Nb and Sn in nuclear-grade zirconium alloys by inductively coupled plasma atomic emission spectrometry using matrix matching was established. The major elements such as Fe, Ni, Nb and Sn were successfully determined by matrix matching with high-purity sponge zirconium and the best experiment of sample solution. The recoveries of Fe, Ni, Nb and Sn in two different samples were between 98.5% to 99.5%, 102% to 104%respectively. The relative standard deviations were all less than 2%(n=10), which met the requirement of Westinghouse certification standard. The linear correlation coefficients were 0.999 9 when the mass concentration of Fe and Ni were 0-10mg/L and the mass concentration of Nb and Sn were 0-100 mg/L. The limits of detection Fe, Ni, Nb and Sn were 2.29, 1.21,1.83, 58.7 μg/g, respectively. The lower limits of determination of Fe, Ni, Nb and Sn were 7.62, 4.04, 6.11, 196 μg/g,respectively.

关 键 词：电感耦合等离子体原子发射光谱法 核级锆合金 标准物质 基体匹配 

分 类 号：O657.31[理学—分析化学]