高温合金中多元素辉光放电质谱法测定及干扰校正

Determination of multi-elements in superalloy by glow discharge mass spectrometry and interference correction

通过辉光放电质谱法(GDMS)测定了高温合金中的C,Mg,Al,P,S,Ti,V,Cr,Mn,Fe,Co,Cu,Nb,Mo,W共15种元素。对辉光放电参数如电流、电压、预溅射时间进行了优化;对高温合金中的质谱干扰进行了分析并详细叙述了各分析元素的干扰情况。选择丰度大且不受干扰或干扰少的同位素用于分析,大多数元素测定结果很好。对于仍存在干扰的元素通过数学校正的方法进行质谱干扰校正。建立干扰校正公式,成功地消除了62Ni2+和36Ar12C+对31P+和48Ti+的质谱干扰。在优化的实验条件下,建立工作曲线。直接对2块高温合金标准样品进行测定,分析结果与认定值吻合,大部分元素的相对标准偏差(RSD)小于5%。

Fifteen elements i.e. C, Mg, Al, P, S, Ti, V, Cr, Mn, Fe, Co, Cu, Nb, Mo and W in superalloy were determined by glow discharge mass spectrometry （GDMS）. The glow discharge parameters such as current, voltage, and pre-burn time were optimized. The mass interferences in superalloy were analyzed,and the interferences of analysis isotopes were described in detail. After isotopes with high abundance, non-interference or light interference were selected for analysis, most elements could be determined very well, while for the elements which are still interfered a mathematic correction method was used to correct the mass spectral interferences. Correction formulas were established in this experiment, and then the mass spectral interferences of 62^Ni^2＋ and 36^Ar^12C^＋ to 31^p^＋ and 48^Ti^＋ have been removed successfully. Under the optimized experiment conditions, the calibration curves were established, and two pieces of superalloy standard samples were directly determined. The analysis results were close with certified values of standard samples, moreover, the relative standard deviations （RSDs） of most elements were less than 5 %.