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辉光放电质谱法测定镍基高温合金中痕量镉

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辉光放电质谱(GDMS)测定镍基高温合金中痕量镉时,会受到114Sn+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(RSFstd)先进行校正后再采用干扰校正方程校正114Sn+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48 mA,放电气体流速为450 mL/min,预溅射时间为20 min.采用镉认证值小于0.1 μg/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0.081 μg/g和0.27 μg/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.
Determination of trace cadmium in nickel-based superalloy by glow discharge mass spectrometry
When glow-discharge mass spectrometry(GDMS)is used to determine trace cadmium in nickel-based superalloy,it is interfered by 114Sn+and MoO+polyatomic ions.After pre-correction with standard relative sensitivity factor(RSFstd),the mass spectral interferences of multi-atomic ions including 114Sn+and MoO+were corrected by interference correction equation.Thus,a method for determination of trace cad-mium in nickel-based superalloy was realized by GDMS at high-resolution mode with 114Cd as analytical iso-tope.The instrument parameters were optimized as follows:the discharge current was 48 mA;the flow rate of discharge gas was 450 mL/min;the pre-sputtering time was 20 min.The certified reference materi-als of nickel-based wrought superalloy with Cd certified value less than 0.1 μg/g and Mo mass fraction of 3%were used as blank samples and determined for 11 times 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 0.081 μg/g and 0.27 μg/g,respectively.The content of cadmium in certified reference ma-terial 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 devi-ations(RSD,n=6)were less than 12%.The contents of cadmium in 3 nickel-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.

glow discharge mass spectrometry(GDMS)nickel-based superalloycadmiummolybdenum

欧阳宇、胡净宇、邵秋文、侯艳霞、杨国武

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钢铁研究总院有限公司,北京 100081

钢研纳克检测技术股份有限公司,北京 100081

辉光放电质谱法(GDMS) 镍基高温合金

2024

冶金分析
中国钢研科技集团有限公司(钢铁研究总院) 中国金属学会

冶金分析

CSTPCD北大核心
影响因子:1.124
ISSN:1000-7571
年,卷(期):2024.44(12)