电感耦合等离子体-原子发射光谱测定再生加氢催化剂中活性组分Mo、Ni及金属杂质

Determination of the Active Component Mo and Ni Content in Regeneration Hydro-Catalyst by ICP-AES

针对再生加氢催化剂中残余的积炭对活性金属含量测定的影响，建立了一种以硝酸-高氯酸体系溶解样品，电感耦合等离子体原子发射光谱（ICP-AES）测定再生加氢催化剂中活性金属Mo、Ni含量的方法。该方法亦可同时测定运转过程中沉积在催化剂表面的金属杂质Fe、Na、Ca、Mg的含量。实验考察了仪器工作参数、不同预处理方法、介质酸度、基体A1对测量结果的影响。本法对Mo、Ni、Fe、Na、Ca、Mg6种元素的检出限分别为0．1797、0．0026、0．0014、0．0220、0．0022、0．0013μg／g，回收率在95％～107％之间。该法准确、可靠，精密度好，可用于实际样品分析。

In order to solve the problem of the effects of remnant carbon build-up in regeneration hydro-catalyst on active metal content measurement, a method of inductively coupled plasma atomic emission spectrometry （ICP-AES） with HNO3-HClO4 wet digestion has been developed. This method can also be used for the measurement of the metal impurity Fe,Na, Ca, and Mg contents in catalyst surface, The effects of medium acidity and matrix effect are studied. The detection limits are 0. 1797 μg/g for Mo, 0. 0026 μg/g for Ni, 0. 0014 μg/g for Fe, 0. 0220 μg/g for Na,0. 0022 μg/g for Ca, and 0. 0013 μg/g for Mg. The recovery for the spiked sample is in the range of 95%～105%. The developed method is precise, accurate, reliable, and could be used for the pratical analysis.