超级微波消解-ICP-AES法测定铑炭催化剂中铑含量

Determination of rhodium content in rhodium carbon catalyst by super microwave digestion and ICP-AES

建立一种采用超级微波消解,ICP光谱法测定5%Rh/C催化剂中Rh含量的方法。通过单因素实验和正交优化,对称样量、酸体系、消解温度、消解时间等因素进行考察,确定最佳消解方法:约0.10 g试样在密闭消解罐中,以9 mL硝酸和1 mL过氧化氢为酸体系,240℃消解温度下保持40 min,经赶酸定容后,采用ICP-AES法测定溶液中的贵金属含量。该方法简便、快捷,消解试样完全且结果稳定,相对标准偏差小于1.0%。

A method for the determination of rhodium content in 5%rhodium carbon catalyst by super microwave digestion and ICP spectroscopy was established.Through single factor experiment and orthogonal optimization,the weighing sample,acid system,digestion temperature,digestion time were investigated.The optimal digestion conditions were determined that the 0.10 g samples were stored in a closed digestion tank with 9.0 mL HNO 3 and 1.0 mL H 2 O 2 as acid system,the samples were kept at 240℃for 40 min.After acid removal and volume determination,the content of precious metals in the solution was determined by ICP-AES method.The method is simple and fast,the samples digestion are complete and the results are stable,the relative standard deviation is less than 1.0%.