ICP-MS/MS测定镍基高温合金中痕量金、汞和硒的质谱干扰消除  

Interference removal in mass spectrometry for the determination of trace gold,mercury and selenium in nickel-based superalloys by ICP-MS/MS

作　　者：王昭颖 陈雄飞 徐彦[3] 墨淑敏 张芳 童坚 刘英 WANG Zhaoying;CHEN Xiongfei;XU Yan;MO Shumin;ZHANG Fang;TONG Jian;LIU Ying(Guobiao(Beijing)Testing&Certification Co.,Ltd.,National Analysis and Testing Center of Nonferrous Metals and Electronic Materials,Beijing 101407,China;Beijing General Research Institute for Nonferrous Metals,Beijing 100088,China;China National Accreditation Service for Conformity Assessment,Beijing 100062,China)

机构地区：[1]国标(北京)检验认证有限公司,国家有色金属及电子材料分析测试中心,北京101407 [2]北京有色金属研究总院,北京100088 [3]中国合格评定国家认可中心,北京100062

出　　处：《分析试验室》2024年第8期1183-1189,共7页Chinese Journal of Analysis Laboratory

基　　金：工信部“航空发动机及燃气轮机重大专项基础研究项目”(HT-J2019-VI-0023-0140)资助。

摘　　要：采用单四极杆质谱(ICP-MS)无法消除第二代镍基单晶高温合金CMSX-4中合金元素Ta,W,Ni及载气Ar所形成的多原子离子对痕量杂质元素Au,Hg和Se产生的质谱干扰。本研究基于三重四极杆-电感耦合等离子体质谱(ICP-MS/MS)技术,通过考察不同碰撞/反应模式(No Gas模式、He模式、O_(2)原位质量模式、O_(2)质量转移模式)下的质谱干扰消除效果,建立了CMSX-4中痕量杂质元素Au,Hg和Se的测定方法。结果表明,采用O_(2)原位质量模式能够有效消除Ta O^(+)对Au^(+)和WO^(+)对Hg^(+)的质谱干扰;采用O_(2)质量转移模式能够消除Ni O^(+)和ArAr^(+)对Se^(+)的质谱干扰。综合考虑3种待测元素的信号强度及背景等效浓度,确定O_(2)流速为0.60 m L/min。通过考察内标元素对基体效应的校正效果,选择^(133)Cs为测定Au和Hg的内标元素、^(103)Rh为测定Se的内标元素。在优化条件下,建立了Au,Hg和Se的工作曲线,线性相关系数均为0.9991,方法检出限为0.11~0.29 ng/m L。分别对3个添加水平的镍基高温合金样品独立测定9次,相对标准偏差(RSD)为2.0%~9.5%。Au和Hg的加标回收率为96.1%~107.2%。采用本方法对镍基高温合金有证标准物质中的Se的质量浓度进行测定,经t检验表明测定结果与标准值无显著性差异。The traditional single-quad inductively coupled plasma mass spectrometry(ICP-MS)cannot eliminate the mass spectrometry interference caused by the polyatomic ions formed by Ta,W and Ni elements and carrier gas Ar in the determination of trace impurity elements Au,Hg and Se in the second-generation nickel-based single crystal high-temperature alloy CMSX-4.Based on triple quadrupole-inductively coupled plasma mass spectrometry(ICP-MS/MS)technology,the working conditions of the instrument were studied by investigating the effects of mass spectrum interference cancellation under different collision or reaction modes(No Gas mode,He mode,O_(2)on-mass mode,and O_(2)mass-shift mode).A method was established for the determination of trace impurity elements Au,Hg and Se in CMSX-4.The results showed that the mass spectrometry interference of TaO^(+)on Aut and WO^(+)on Hg^(+)can be effectively eliminated by using O_(2)on-mass mode;the mass spectrometry interference of NiO^(+)and ArAr^(+)on Se can be effectively eliminated by using O_(2)mass-shift mode.Considering the signal intensities and background equivalent concentrations of the 3 elements to be measured,the O_(2)flow rate was determined to be 0.60 mL/min.Also,^(133)Cs was selected as the internal standard element for the measurement of Au and Hg,while^(103)Rh was selected for the measurement of Se after comparing the effects of correcting matrix effects and analyte signal drift by internal standard elements.The linear equations of Au,Hg and Se have been established under the optimal conditions,and the linear correlation coefficients were 0.9991.The detection limits of Au,Hg,and Se were 0.11-0.29 ng/mL.The relative standard deviations(RSDs)were 2.0%-9.5%,and the spiked recoveries of Au and Hg were 96.1%-107.2%by determining the samples of 3 supplemental levels and the recoveries of the bidding recycling of 9 groups.The results showed no significant difference between the identification value by t-test of Se in the standard substance in the nickel-based high-temperature al

关 键 词：三重四极杆-电感耦合等离子体串联质谱(ICP-MS/MS) CMSX-4镍基单晶高温合金 痕量杂质元素 质谱干扰消除 

分 类 号：O657.31[理学—分析化学] X832[理学—化学]