采用电感耦合等离子体质谱法测定镍基高温合金中锗、砷、钇、钌、铟、碲、铪、铂、金、汞等10种元素。样品以盐酸-硝酸混合酸溶解,并在完全溶解后滴加过氧化氢防止生成钨酸沉淀。在测定中采用基体匹配法和在线内标法校正基体效应和进样不均匀导致的信号扰动。待测元素的质谱干扰通过选择合适的同位素、加入元素修正方程和在测试中应用动能碰撞模式来进行消除。10种元素的检出限(3s)在0.002~0.65 μg·g-1之间。应用此方法分析了3个标准样品(GBW 01636,GBW 01638,GBW 01640),测定值与认定值相符,测定值的相对标准偏差(n=10)在0.60%~45%之间。

ICP-MS was applied to the determination of 10 elements i.e. Ge, As, Y, Ru, In, Te, Hf, Pt, Au and Hg in nickel base superalloy. The sample was digested with a mixture of hydrochloric acid and nitric acid. Hydrogen peroxide was added after digestion in order to avoid precipitation of tungstic acid. In testing, methods of matrix matching and on-line internal standard were applied to compensate the signal disturbance caused by matrix effect and sampling rate. The mass spectrum interference was eliminated by choosing proper isotope, using correction equation and applying kinetic energy bias mode. Detection limits (3s) of the 10 elements found were in the range of 0.002-0.65 μg·g-1. The proposed method was used in the analysis of 3 standard samples (GBW 01636, GBW 01638 and GBW 01640), giving results in consistency with the certified value with RSD′s (n=10) in the range of 0.60%-45%.