高分辨电感耦合等离子体质谱法测定镍基高温合金中的痕量元素  

Determination of Trace Elements in Nickel-based High-temperature Alloy by High Resolution Plasma Mass Spectrometry

作　　者：胡璇 王昭颖 陈雄飞 程紫辉 张英新 王倩[2] 侯可军[2] HU Xuan;WANG Zhao-ying;CHEN Xiong-fei;CHENG Zi-hui;ZHANG Ying-xin;WANG Qian;HOU Ke-jun(Guobiao(Beijing)Testing&Certification Co.,Ltd,Beijing 100088,China;Institute of Mineral Resources,Chinese Academy of Geological Sciences,Beijing 100089,China)

机构地区：[1]国标(北京)检验认证有限公司,北京100088 [2]中国地质科学院矿产资源研究所,北京100089

出　　处：《质谱学报》2023年第4期556-566,I0005,共12页Journal of Chinese Mass Spectrometry Society

基　　金：国家科技重大专项(J2019-Ⅵ-0023-0140)。

摘　　要：本研究建立了高分辨电感耦合等离子体质谱(HR-ICP-MS)法测定镍基高温合金中痕量元素。采用盐酸、硝酸和氢氟酸溶解镍基高温合金样品,根据待测元素同位素丰度大、干扰小、灵敏度高的原则,优化各待测元素的同位素和分辨率,有效消除了绝大多数多原子和双电荷离子的干扰。另外,考察了基体、合金成分和溶样酸对待测痕量元素的质谱干扰,通过选取合适的内标133Cs,可以克服基体效应并降低信号漂移。利用甲基异丁基酮萃取Cd,萃取效率达99.7%,消除了镍基高温合金中主成分Mo的质谱干扰。各痕量元素校准曲线的线性相关系数均大于0.999,方法检出限为0.0021~0.074μg/g。用本方法分析镍基高温合金成分分析标准物质中的痕量元素含量,测定结果的相对标准偏差(RSD,n=6)在2.9%~7.8%之间,测定值与标准值非常接近。该方法前处理简单、分析速度快、结果准确可靠,能够满足镍基高温合金中痕量元素的检测需求。The nickel content of nickel-based high-temperature alloy is between 50%and 70%,and the alloy contents of chromium,iron,cobalt,molybdenum,aluminum,titanium and tungsten are within 20%.A method of high resolution plasma mass spectrometry was established to determine the trace elements in nickel-based high-temperature alloy.According to the principle of large isotope abundance,small interference and high sensitivity,the isotopes and resolution of the elements to be measured were optimized,the interferences of most of the multi-atom and double-charged ions were effectively eliminated.The mass spectral interferences of matrix,compositions of alloy and dissolving acid on the trace elements were investigated.The appropriate internal standard of caesium was selected to overcome the matrix effect and reduce the signal drift.Chromium was extracted by methylisobutylone,the extraction efficiency reached up to 99.7%,which eliminated the mass spectral interference of principal component molybdenum in the nickel-based high-temperature alloy.The linear correlation coefficient of the calibration curve was greater than 0.999,and the method detection limit was between 0.0021 and 0.074μg/g.The trace elements in the reference material was analyzed,the relative standard deviation(RSD,n=6)was between 2.9%and 7.8%,and the measured value was very consistent with the standard value.This method is simple,fast,accurate and reliable,which can meet the requirement of trace elements determination in nickel-based high-temperature alloy.

关 键 词：高分辨电感耦合等离子体质谱(HR-ICP-MS) 镍基高温合金 痕量元素 

分 类 号：O657.63[理学—分析化学]