建立了氨水络合分离-电感耦合等离子体质谱法（ICP-MS）测定含Ta和Hf的单晶高温合金中痕量Au的方法。在样品中加入体积比为3∶1的盐酸-硝酸混合溶液，于60℃加热30 min。滴加氨水至溶液酸度达到pH 9.0，用于沉淀Ta和Hf及络合Au。静置30 min后，用滤纸过滤，向滤液中加入50%（体积分数）硝酸溶液，用水定容至50 mL，用四极杆电感耦合等离子体质谱仪在射频功率为1 350 W和雾化器流量为0.70 L·min^-1条件下测定溶液中的Au含量，用基质匹配标准溶液系列制作标准曲线。结果显示：在不进行氨水络合分离时，HfOH⁺、TaO⁺在质荷比（m/z）196.9附近产生质谱峰会干扰Au⁺的测定，高温合金中的Hf与Ta的质量分数分别在0.01%~2.00%和0.05%~10.00%内与其产生的HfOH⁺与TaO⁺干扰量呈线性关系，且干扰量远大于合金中的含Au量（0.1 μg·g^-1水平），无法用干扰量的线性回归方程扣除。Au的质量分数在0.1~10.0 μg·g^-1内与其对应响应值呈线性关系，检出限（3s）为0.002 μg·g^-1。对实际样品进行加标回收试验，测定值的相对标准偏差（n=6）均小于10%，回收率为101%~110%，且测定值和ISO/TS 15338：2009（E）中辉光放电质谱法（GD-MS）的基本一致。

A method for the determination of trace Au in single crystal superalloys containing Ta and Hf was established by inductively coupled plasma mass spectrometry (ICP-MS) after complexing separation with ammonia. The sample was dissolved by a mixed solution of hydrochloric acid and nitric acid with a volume ratio of 3:1 at 60℃ for 30 min. To precipitate Ta and Hf and complex Au for determination, the acidity of the solution was adjusted to pH 9.0 with adding ammonia dropwise. After keeping under steady condition for 30 min, the solution was passed through filter paper. 50% (volume fraction) nitric acid solution was added and the volume of the solution was made up to 50 mL with water. The content of Au in the solution was determined by quadrupole-ICP-MS at the radio-frequency powder of 1 350 W and argon flow rate of 0.70 L·min^-1, and the standard curve was made with the matrix matching standard solution series. The results showed that when ammonia complex separation was not adopted, the determination of Au would be interfered by the mass peak of HfOH⁺ and TaO⁺ at the m/z about 196.9, the mass fractions of Hf (0.01%-2.00%) and Ta (0.05%-10.00%) in superalloy were linearly related with the interference amounts of HfOH⁺ and TaO⁺ respectively, and the interference amount was much larger than the Au content in alloy (0.1 μg·g^-1), which cannot be deducted by the linear regression equation of the interference. Linearity relationship between mass fractions of Au and corresponding response values was kept in the range of 0.1-10.0 μg·g^-1, with detection limit (3s) of 0.002 μg·g^-1. The spiked recovery test was made on the actual samples, values of recovery of Au was found in the range of 101%-110%, with RSDs (n=6) of the determined values less than 10%, and the determined values of the prescribed method was in conformity with those of glow discharge mass spectrometry (GD-MS) from ISO/TS 15338:2009(E).