电感耦合等离子体质谱法测定金属铍珠中痕量杂质元素  

Determination of trace impurity elements in beryllium metal pebble by inductively coupled plasma mass spectrometry

作　　者：郭文韬 王雷 孟祥娥 方哲 王超刚 王瑞 GUO Wentao;WANG Lei;MENG Xiang’e;FANG Zhe;WANG Chaogang;WANG Rui(NCS Testing Technology Co.,Ltd.,Beijing 100094,China)

机构地区：[1]钢研纳克检测技术股份有限公司,北京100094

出　　处：《冶金分析》2023年第9期28-34,共7页Metallurgical Analysis

基　　金：国家重点研发计划(2021YFF0700103)。

摘　　要：铍中杂质元素的含量直接影响铍材的各种性能,准确测定其含量具有重要意义。用盐酸-硝酸体系溶解样品,以标准模式测定同位素^(7)Li、^(114)Cd、^(147)Sm、^(153)Eu、^(157)Gd、^(163)Dy,控制氦气流量为6.0mL/min,在氦气碰撞池动能歧视(KED)模式下测定^(27)Al、^(52)Cr、^(55)Mn、^(56)Fe、^(60)Ni、^(208)Pb,建立了电感耦合等离子体质谱法(ICP-MS)测定铍珠中锂、铝、铬、锰、铁、镍、镉、钐、铕、钆、镝、铅12种痕量杂质元素的分析方法。考察了基体效应,确定采用逐级稀释样品溶液以降低基体浓度和在线加内标校正这两种方法克服基体效应。考虑到铍珠中铁、铝杂质的含量要比其余杂质元素含量高,使用稀释因子为200的试液测试铁、铝杂质元素含量,其余元素含量使用稀释因子为50的试液进行测试。采用内标45Sc校正锂、铝、铬、锰、铁、镍,内标103 Rh校正镉、钐,内标187 Re校正铕、钆、镝、铅。实验表明,各待测元素校准曲线的线性相关系数均大于0.9995,方法检出限为0.002~2.90μg/g,定量限为0.006~9.67μg/g。将实验方法用于纯度牌号为Be-2的金属铍珠样品中锂、铝、铬、锰、铁、镍、镉、钐、铕、钆、镝、铅这12种痕量元素的测定,并进行加标回收试验,结果的相对标准偏差(RSD,n=6)为0.76%~7.0%,加标回收率95%~118%;采用标准GJB 2513A—2008进行方法对照试验,实验方法与标准方法测定结果的绝对误差均在标准方法规定的允许差范围内。The content of impurity elements in beryllium directly affects the properties of beryllium materials.The accurate determination of their contents is of great significance.The beryllium metal pebble sample was dissolved in hydrochloric acid-nitric acid system.The isotopes of^(7)Li,^(114)Cd,^(147)Sm,^(153)Eu,^(157)Gd and^(163)Dy were determined at standard mode,and^(27)Al,^(52)Cr,^(55)Mn,^(56)Fe,^(60)Ni and^(208)Pb were determined at the mode of helium collision cell kinetic energy discrimination(KED)with helium flow rate of 6.0mL/min.Thus,a method for determination of twelve trace impurity elements(Li,Al,Cr,Mn,Fe,Ni,Cd,Sm,Eu,Gd,Dy and Pb)in beryllium metal pebble by inductively coupled plasma mass spectrometry(ICP-MS)was established.The matrix effect investigated,and it was overcome through stepwise dilution of sample solution to reduce the matrix concentration and online correction with internal standard.Considering that the contents of Fe and Al in beryllium metal pebble were higher than other impurity elements,the sample solution with dilution factor of 200was used for determination of Fe and Al,while the dilution factor of 50was used for determination of other elements.The internal standard of 45Sc was used to correct Li,Al,Cr,Mn,Fe and Ni.The internal standard of 103 Rh was used to correct Cd and Sm.The internal standard of 187 Re was used to correct Eu,Gd,Dy and Pb.The experimental results showed that the linear correlation coefficients of calibration curves for elements were all higher than 0.9995,the limits of detection were 0.002-2.90μg/g,and the limits of quantification were 0.006-9.67μg/g.The proposed method was applied for determination of twelve trace impurity elements(Li,Al,Cr,Mn,Fe,Ni,Cd,Sm,Eu,Gd,Dy and Pb)in beryllium metal pebble sample with purity grade of Be-2.Moreover,the standard addition recovery tests were conducted.The relative standard deviations(RSD,n=6)of determination results were between 0.76%and 7.0%,and the recoveries were between 95%and 118%.The standard method of GJB 2513A-2008wa

关 键 词：金属铍珠 电感耦合等离子体质谱法(ICP-MS) 基体效应 动能歧视碰撞池(KED) 

分 类 号：O675.63[理学—化学] TF146.24[冶金工程—冶金物理化学]