ICP-AES法测定丙烯腈催化剂中活性组分钼和铋

ICP-AES Method for the Determination of Active Components Mo and Bi in Catalyst for Acrylonitrile Production

报道用ICP AES法测定丙烯腈催化剂中的活性组分钼和铋。催化剂试样 0 2g在 75℃低温下溶于 5mL王水 ,8mL氢氟酸 ,蒸干驱除SiF4。用 3%盐酸溶解剩余试样至澄清 ,并定容于 1 0 0mL容量瓶中 ,用于测定Bi,再用 3%盐酸稀释 1 0倍 ,用于测定Mo。由分析线轮廓描迹和空白、共存物在分析线附近的扫描观察分析线的光谱干扰 ,在此基础上选用不受光谱干扰的分析线BiⅡ 1 90 2 4 1nm ,BiⅠ 2 2 3 0 6 1nm ,MoⅡ 2 0 2 0 30nm ,MoⅡ 2 0 3 84 4nm ,MoⅡ 2 0 4 5 98nm。在全谱记录的光谱中同一元素采用多条分析线同时测定有利于改善分析数据的准确度和精确度。方法成功用于丙烯腈生产中监测催化剂活性。

An ICP AES method for the determination of active components Mo and Bi in catalyst for acrylonitrile production was established and reported in this paper. 0 2 g of the sample was dissolved with 5 mL of aqua regia and 8 mL of HF at 75 ℃ on a water bath and evaporated till dry to expel SiF 4. The residue was dissolved and made volume with 3% HCL up to 100 mL. The soution was prepared for Bi determination. Successively diluted with 3% HCL for 10 times the solution was used for Mo determination. Spectral interferences were investigated in detail by means of profiling the analytical lines with wavelength scanning of the blank and coexisting elements in the vicinity of the lines. Three Mo lines, MoⅡ202 030, MoⅡ203 844 and MoⅡ204 598, and two Bi lines, BiⅡ190 241 and BiⅠ223 061 were selected as the analytical lines considered free of spectral interferences. Utilizing multiple lines in a full spectrum for simultaneous determination of one element is of benefit to the improvement of accuracy and precision of the analysis. The method has been successfully used for monitoring the activity of the catalyst in acrylonitrile production.