【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¹¹⁴Sn⁺及MoO⁺多原子离子的质谱干扰。本文选择¹¹⁴Cd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0.1μg/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。更多还原

【Abstract】 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(RSF_Std), 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 cadmium in nickel-based superalloy was realized by GDMS at high-resolution mode with ¹¹⁴Cd as analytical isotope. 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 materials 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 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 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.更多还原