高分辨辉光放电质谱定量分析变形高温合金GH4169中29种杂质元素  

Quantitative analysis of 29 impurity elements in deformed superalloy GH4169 by high resolution glow discharge mass spectrometry

作　　者：侯艳霞[1,2] 乔丽丽 王雷 杨国武[2] 胡净宇 李小佳 HOU Yanxia;QIAO Lili;WANG Lei;YANG Guowu;HU Jingyu;LI Xiaojia(Central Iron and Steel Research Institute Co.,Ltd.,Beijing 100081,China;NCS Testing Technology Co.,Ltd.,Beijing 100081,China)

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

出　　处：《冶金分析》2024年第7期1-8,共8页Metallurgical Analysis

基　　金：国家重点研发计划项目(2021YFF0700105)。

摘　　要：变形高温合金GH4169广泛用于航空、航天、能源等领域,其中的杂质元素直接影响其性能、品质及服役寿命,建立多种杂质元素同时、快速、准确的分析方法对于GH4169合金的应用具有重要意义。本文采用高分辨辉光放电质谱(GDMS)定量分析了变形高温合金GH4169中29种杂质元素,通过优化辉光放电质谱参数,探讨了辉光电离过程中放电参数对待测元素灵敏度的影响,确定了实验条件:放电电压850 V,放电电流50 mA,气体流速450 mL/min。考察了待测元素的质谱干扰情况,选择相对丰度高、干扰少的同位素在不同的分辨模式(中/高)进行测试。使用基体匹配的标准物质或控制样品校准29种待测元素的相对灵敏度因子(RSF),实现了对变形高温合金GH4169中镁、磷、砷、铅等29种杂质元素的定量分析。采用实验方法对GH4169合金样品进行测定,同时采用可溯源的电感耦合等离子体原子发射光谱法(ICP-AES)、高频感应燃烧红外吸收法、氢化物发生-原子荧光光谱法(HG-AFS)、电感耦合等离子体质谱法(ICP-MS)等进行结果比对;采取t检验对测试结果进行准确性检验,其中28种元素(除Cd外)测定结果的t检验值为0.500~2.300.025,8=2.306,在95%置信区间内,GDMS测试结果与以上分析方法结果无显著性差异,Cd采用GDMS测定的结果和三重四极杆-电感耦合等离子体质谱法(ICP-MS/MS)测定结果一致;29种杂质元素测定结果的相对标准偏差(RSD,n=6)在1.0%~25.7%之间。Deformed superalloy GH4169 is widely used in aviation,aerospace and energy fields.The impurity elements in alloy can directly affect its performance,quality and service life.Therefore,the establishment of simultaneous,fast and accurate analytical method for a variety of impurity elements has great significance for the application of GH4169 alloy.In this study,glow discharge mass spectrometry(GDMS)was employed for the quantitative analysis of 29 impurity elements in the deformed superalloy GH4169.By optimizing the parameters of GDMS,the influence of discharge parameters in glow ionization on the sensitivity of measured elements was discussed.The experimental conditions were obtained as follows:the discharge voltage was 850 V,the discharge current was 50 mA,and the gas flow was 450 mL/min.The mass spectrometry interference of measured elements was investigated,and the isotopes with high relative abundance and low interference were selected for testing in different resolution modes(medium/high).The relative sensitivity factors(RSF)of 29 impurity elements were calibrated using matrix-matched certified reference materials or control samples.The quantitatively analysis of 29 impurity elements such as magnesium,phosphorus,arsenic,and lead in deformed superalloy GH4169 was realized.The GH4169 alloy sample was determined according to the experimental method.Meanwhile,the traceable inductively coupled plasma atomic emission spectrometry(ICP-AES),high frequency induction combustion infrared absorption method,hydride generation-atomic fluorescence spectrometry(HG-AFS)and inductively coupled plasma mass spectrometry(ICP-MS)were used for comparison.The accuracy of measurement results was verified by t test.The t-test value of the determination results of 28 impurity elements(except for Cd)was 0.500-2.30.

关 键 词：高分辨辉光放电质谱(GDMS) 定量分析 变形高温合金GH4169 杂质元素 

分 类 号：O657.31[理学—分析化学] TF125.12[理学—化学]