基于磷钼蓝反应测定钴-钼催化剂浸渍液中钼离子含量  

Determination of Molybdenum Ion in Impregnation Solution of Co-Mo Catalysts Based on the Reaction of Phosphorus Molybdenum Blue

作　　者：杜鑫[1] 李永生[1] 

机构地区：[1]四川大学化学工程学院,成都610065

出　　处：《理化检验（化学分册）》2015年第3期296-299,共4页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

摘　　要：基于磷钼蓝反应测定钴-钼催化剂浸渍液中钼离子含量。建立了一个流动注射-磷钼蓝分光光度法测定高浓度钼离子的含量,优化后的条件为:1酸度调节剂为0.5mol·L-1硫酸溶液;2载流为超纯水;3反应试剂为120g·L-1磷酸二氢钾、100g·L-1抗坏血酸及0.3mol·L-1硫酸的混合液;4总流量为2.8 mL·min-1;5酸度调节盘管长度为20cm;6反应盘管长度为250cm。三氧化钼的质量浓度在10.0~300.0g·L-1范围内与峰高呈线性关系,检出限(3s/k)为2.0g·L-1。方法用于钴-钼催化剂钼浸渍液的分析,回收率在99.7%~105%之间,测定值的相对标准偏差(n=11)小于1%。Molybdenum ion in impregnation solution of Co-Mo catalysts was determined based on reaction of phosphorus molybdenum blue.A system for measuring high molybdenum ion concentration was established based on the spectrophotometry of flow injection-phosphorus molybdenum blue.The optimized conditions of the system found were as follows:1 acidity regulator:0.5 mol·L-1 H2SO4 solution;2 carrier:ultrapure water;3 reaction reagent:mixture of 120g·L-1 KH2PO4,100g·L-1 Vc and 0.3mol·L-1 H2SO4;4total flow rate:2.8mL·min-1;5length of acidity adjusted coil:20cm;6length of reaction coil:250cm.The linear relationship between values of the peak height and the mass concentration of MoO3 was obtained in the range of 10.0-300.0g·L-1,with detection limit(3s/k)of 2.0g·L-1.The proposed method was applied to the analysis of samples of impregnation solution of Co-Mo catalysts,giving recovery rates in the range of 99.7%-105% with RSD′s(n=11)less than 1%.

关 键 词：分光光度法 磷钼蓝 钼离子 钴-钼催化剂 浸渍液 

分 类 号：O657.3[理学—分析化学] TQ426[理学—化学]