辉光放电质谱法测定镍基高温合金中痕量镉  

Determination of trace cadmium in nickel-based superalloy by glow discharge mass spectrometry

作　　者：欧阳宇[1,2] 胡净宇 邵秋文[2] 侯艳霞 杨国武 OUYANG Yu;HU Jingyu;SHAO Qiuwen;HOU Yanxia;YANG Guowu(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12期1-6,共6页Metallurgical Analysis

基　　金：国家重点研发计划(2021YFF0700105);国家重点研发计划(2021YFB3700405)。

摘　　要：辉光放电质谱(GDMS)测定镍基高温合金中痕量镉时,会受到^(114)Sn^(+)及MoO^(+)多原子离子的质谱干扰。本文选择^(114) Cd为分析同位素和高分辨模式,采用标准相对灵敏度因子(RSF_(Std))先进行校正后再采用干扰校正方程校正^(114)Sn^(+)及MoO^(+)多原子离子的质谱干扰,实现了辉光放电质谱对镍基高温合金中痕量镉的测定。对仪器参数进行了优化,确定参数如下:放电电流为48mA,放电气体流速为450mL/min,预溅射时间为20min。采用镉认证值小于0.1μg/g、钼质量分数为3%的镍基变形高温合金标准样品作为空白样品,连续测定11次,以3倍空白标准偏差和10倍空白标准偏差分别计算得到检出限和定量限为0.081μg/g和0.27μg/g。采用实验方法测定镍基变形高温合金标准样品中镉含量,测定结果与认定值/标准值吻合性较好,相对标准偏差(RSD,n=6)小于12%。采用实验方法和电感耦合等离子体串联质谱法(ICP-MS/MS)分别对3种镍基高温合金样品中的镉含量进行测定,结果表明,两种方法测定结果基本一致。When glow-discharge mass spectrometry(GDMS)is used to determine trace cadmium in nickelbased superalloy,it is interfered by ^(114)Sn^(+)and MoO^(+)polyatomic ions.After pre-correction with standard relative sensitivity factor(RSF_(Std)),the mass spectral interferences of multi-atomic ions including ^(114)Sn^(+)and MoO^(+)were corrected by interference correction equation.Thus,a method for determination of trace cadmium in nickel-based superalloy was realized by GDMS at high-resolution mode with ^(114)Cd as analytical isotope.The instrument parameters were optimized as follows:the discharge current was 48mA;the flow rate of discharge gas was 450mL/min;the pre-sputtering time was 20min.The certified reference materials of nickel-based wrought superalloy with Cd certified value less than 0.1μg/g and Mo mass fraction of 3%were used as blank samples and determined for 11times consecutively.The limit of election and limit of quantifiation,which were calculated according to three-fold and ten-fold of standard deviation of blank sample,were 0.081μg/g and 0.27μg/g,respectively.The content of cadmium in certified reference material or reference material of nickel-based superalloy were determined according to the proposed method,and the results were in good agreement with the certified value/standard value.The relative standard deviations(RSD,n=6)were less than 12%.The contents of cadmium in 3nickel-based superalloy samples were determined according to the proposed method as well as inductively coupled plasma tandem mass spectrometry(ICP-MS/MS),respectively.The results showed that the results of the above two methods were basically consistent.

关 键 词：辉光放电质谱法(GDMS) 镍基高温合金 镉 钼 

分 类 号：O657.63[理学—分析化学] TF031[理学—化学]