高流速高分辨辉光放电质谱法测定粉末高温合金中26种微量和痕量元素

准确测定粉末高温合金中微量及痕量元素,对粉末高温合金的生产、应用具有重要意义。将样品在放电电流40～45 mA,放电电压1 100～1 200 V,氩气流速400～450 mL/min下进行辉光放电激发,选择合适的同位素和分辨率以消除质谱干扰,使用基体匹配的内控标准样品和标准物质校准各待测元素的相对灵敏度因子(RSF),实现了高流速高分辨辉光放电质谱法(GDMS)对粉末高温合金中硼、钠、镁等26种微量及痕量元素的测定。采用实验方法对粉末高温合金内控样品中26种微量及痕量元素进行测定,各待测元素的测定值与参考值基本一致,测定结果的RSD(n=6)在0.9%～15.4%之间。采用实验方法对粉末高温合金样品进行测定,测定结果分别与电感耦合等离子体原子发射光谱法(ICP-AES)测定硼、铁和锆,高频感应燃烧红外吸收法测定硫,原子荧光光谱法测定硒,高分辨电感耦合等离子体质谱法(HR-ICP-MS)测定其余元素(钠、镁、硅、磷、钙、钒、锰、铜、镓、砷、银、锡、锑、碲、镧、铈、铪、钽、铊、铅和铋)的结果保持一致,测定结果的RSD(n=6)在0.2%～26.6%之间。

Determination of twenty-six micro and trace elements in powder metallurgy superalloy by fast-flow and high-resolution glow discharge mass spectrometry

The accurate determination of micro and trace elements in powder metallurgy superalloys is of great significance for the production and application of powder metallurgy superalloys. The glow discharge excitation of samples was carried out at a discharge current of 40-45 mA, a discharge voltage of 1 100-1 200 V and an argon gas flow rate of 400-450 mL/min. Proper isotopes and resolutions were selected to eliminate the mass spectrometry interferences. The relative sensitivity factor (RSF) of each testing element was calibrated using internal control sample and certified reference materials with matrix matching. The determination of 26 micro and trace elements in powder metallurgy superalloy (including B, Na and Mg) by fast-flow and high-resolution glow discharge mass spectrometry (GDMS) was realized. The contents of 26 micro and trace elements in internal control sample of powder metallurgy superalloy were determined according to the experimental method. The found results of each element were basically consistent with the reference values. The relative standard deviations (RSD, n=6) of determination results were between 0.9% and 15.4%. The proposed method was applied for the determination of powder metallurgy superalloy sample, and the found results were consistent with other methods: inductively coupled plasma atomic emission spectrometry (ICP-AES) for B, Fe and Zr; high frequency induction combustion-infrared absorption method for S; atomic fluorescence spectrometry (AFS) for Se; high resolution-inductively coupled plasma mass spectrometry (HR-ICP-MS) for other elements(Na,Mg,Si,P,Ca,V,Mn,Cu,Ga,As,Ag,Sn,Sb,Te,La,Ce,Hf,Ta,Tl,Pb,Bi). The RSDs (n=6) of the results were between 0.2% and 26.6%.