电感耦合等离子体质谱法测定镍基合金中痕量砷、铅、锡、锑  

Determination of Trace Arsenic,Plumbum,Stannum and Stibium in Nickel-Based Alloys by Inductively Coupled Plasma Mass Spectrometry

作　　者：罗凤焱 李文强 张庆宇 王国华[1] 郭晋轩 Luo Fengyan;Li Wenqiang;Zhang Qingyu;Wang Guohua;Guo Jinxuan(Science and Technology on Reactor Fuel and Mateerials Laboratory,Nuclear Power Institute of China,Chengdu,610213,China)

机构地区：[1]中国核动力研究设计院反应堆燃料及材料重点实验室,成都610213

出　　处：《核动力工程》2023年第S02期211-215,共5页Nuclear Power Engineering

摘　　要：为准确测定镍基合金(NBS)中痕量砷、铅、锡、锑,采用电感耦合等离子体质谱法(ICP-MS),于HNO_(3)-HCl体系密闭溶解镍基合金,同位素质量数分别选择75、208、120、121,以动能歧视(KED)模式克服质谱干扰,内标^(89)Y在线监测仪器稳定性和基体效应,建立了NBS中砷、铅、锡、锑的测定方法。在优化条件下,各元素的信号强度与对应质量浓度呈良好的线性关系,线性相关系数大于0.9999,当称样量为0.1 g时,4种元素的检测范围为10.0~100.0μg/g,各元素检测下限均优于0.15 ng/mL,加标回收率在85%~120%之间,加标样品的相对标准偏差(n=6)为2.8%~5.6%。该方法的灵敏度、精密度和准确度良好,可用于NBS中痕量As、Pb、Sn、Sb的测定。In order to accurately determine trace arsenic,plumbum,stannum and stibium in the nickel-based alloy(NBS),inductively coupled plasma mass spectrometry(ICP-MS)was used.The HNO_(3)-HCl system was used for airtight digestion of NBS,and the isotope mass numbers were selected as 75,208,120,and 121 respectively.The kinetic energy discrimination(KED)mode was used to overcome the mass spectral interference,and the internal standard element ^(89)Y was used to monitor the stability of the instrument and the matrix effect online.A method for the determination of arsenic,plumbum,stannum and stibium in nickel-based alloy was established.Under the optimized conditions,the signal intensities of each element had a good linear relationship with the corresponding mass concentrations,and the linear correlation coefficient was greater than 0.9999.When the sample weight was 0.1 g,the detection range of of the four elements was 10.0-200.0μg/g.The detection limit of each element was better than 0.15 ng/mL,and the recovery rate of standard addition was between 85%-120%.The relative standard deviation(n=6)of the spiked sample was 2.8%-5.6%.This method has good sensitity,precision and accuracy,and can be used for the determination of arsenic,plumbum,stannum and stibium in NBS.

关 键 词：镍基合金(NBS) 动能歧视(KED) 电感耦合等离子体质谱法(ICP-MS) 基体效应 

分 类 号：TL34[核科学技术—核技术及应用] O657.63[理学—分析化学] O655.1[理学—化学]