高流速离子源辉光放电质谱校正灵敏度因子法定量分析镍基高温合金中痕量稀土及贵金属元素  

Calibrated Relative Sensitivity Factors for Elemental Quantitative Analysis of Trace Rare Earth&Precious Metal Elements in Nickel Base Superalloy by Glow Discharge Mass Spectrometry with Fast-flow Ion Source

作　　者：屈华阳[1,2] 张馨元 胡净宇 杨国武[2] 王海舟 QU Hua-yang;ZHANG Xin-yuan;HU Jing-yu;YANG Guo-wu;WANG Hai-zhou(Central Iron&Steel Research Institute,Beijing 100081,China;The NCS Testing Technology Co.,Ltd.,Beijing 100081,China)

机构地区：[1]钢铁研究总院,北京100081 [2]钢研纳克检测技术股份有限公司,北京100081

出　　处：《分析测试学报》2024年第9期1317-1323,共7页Journal of Instrumental Analysis

基　　金：国家重点研发计划(2022YFF0609301,2021YFF0700105)。

摘　　要：该文通过全面优化高流速辉光放电离子源分析高温合金痕量元素的仪器条件,系统研究高温合金复杂基体元素造成的质谱干扰,选取稀土元素和贵金属元素分析同位素与合适的质谱分辨率,确立了基于基体匹配的变形高温合金标准物质系列的校正灵敏度因子(RSF)定量方案,使测定结果的相对误差由4.0%~80%优化至7.7%~20%,并为痕量分析结果提供了可靠的计量溯源依据。基于此所建立的辉光放电质谱(GDMS)测定镍基高温合金中稀土元素和贵金属元素的方法检出限为0.0010~0.015μg/g,定量下限为0.0030~0.045μg/g。应用于变形高温合金和铸造高温合金实际样品中稀土元素和贵金属元素的分析,测定结果与湿法分析的参考值吻合较好,较好地验证了辉光放电固体样品快捷分析的优势,体现了高分辨质谱检出限低、线性范围宽、可分析元素多的特点,在高温合金材料质控中有着巨大的应用前景。The experimental conditions of fast-flow glow discharge ion source to analyze the trace ele⁃ments in superalloy were optimized in details.Based on comprehensively investigation on mass spec⁃trometry interferences due to the most complex matrix elements in nickel superalloy,the analytical isotopes and appropriate mass spectrometry resolution for analyze the trace rare earth&precious met⁃al elements were adopted.Relative sensitivity factors calibration scheme,which was calibrated in matched matrix by the homemade wrought superalloy reference material series of gradient content,has been established.Thus the relative error of analysis results was optimized from 4.0%-80%to 7.7%-20%.In addition,the reliable guarantee for metrological traceability of trace analysis has been achieved.The glow discharge mass spectrometry(GDMS)method for determining rare earth ele⁃ments and precious metal elements in nickel base superalloy has been developed with detection limit in 0.0010-0.015μg/g,and quantitative limit in 0.0030-0.045μg/g.The established method was applied to analyze rare earth elements and precious metal elements in actual samples of wrought or cast superalloy,the measurement results are in good agreement with the reference values of wet anal⁃ysis,which verifies the advantages fast treating solid samples by glow discharge,and the characteris⁃tics of high resolution mass spectrometry with low detection limit,wide linear range,and multiple el⁃ements analytical ability.It also shows great application prospects in the quality control of superalloy materials.

关 键 词：辉光放电质谱法 镍基 高温合金 稀土元素 贵金属元素 校正灵敏度因子 

分 类 号：O657.6[理学—分析化学] TG132.3[理学—化学]