ZSM-5催化剂中镍、铜含量的溶出伏安分析  

Determination of Copper and Nickel in ZSM-5 Zeoli Catalyst by Anodic Stripping Voltammetry

作　　者：刘壮[1] 焦玉海[1] 徐丽娟[1] 

机构地区：[1]北京石油化工学院应用化学系,北京102617

出　　处：《分析科学学报》2008年第2期240-242,共3页Journal of Analytical Science

摘　　要：考察了阳极溶出伏安法测定ZSM-5催化剂中Cu^2＋和Ni^2＋的可行性。实验采用玻碳汞膜电极为工作电极的三电极系统，在pH=0．73的0．24mol·L^-1 HCl底液中，Cu^2＋在～0．25V（vs．SCE）附近有一个灵敏的一阶导数溶出峰，其峰高与Cu^2＋在0．01～0．325μg·mL^-1范围内有较好的线性关系，检出限为0．004596μg·mL^-1，相关系数为0．9991，回收率在98．00％～100．5％，精密度在2．27％～5．14％；在pH=9．41的0．06mol·L NH4OH—NH4Cl底液中，Ni^2＋在-0．30V（vs．SCE）附近有一个灵敏的一阶导数溶出峰，此峰高与Ni^2＋在0．5～5．5μg·mL^-1范围内有较好的线性关系，检出限为0．4422μg·mL^-1，相关系数为0．9996，回收率在98．12％～101．7％，精密度在3．64％～6．21％。常见干扰离子Fe^3＋、Zn^2＋、Cd^2＋、Ni^2＋、Al^3＋等对镍和铜的分析无影响。用本法对ZSM-5催化剂中Cu^2＋、Ni^2＋含量进行了测定，获得了满意的结果。A simple,sensitive method for the determination of copper and nickel in ZSM-5 zeoli catalyst by anodic stripping vohammetry has been described. Electrochemical measurements were performed in a three electrode system in which carbon electrode was the working electrode. The favourable concentration of the base solution of copper was 0.24 mol·L^-1 HCl and pH value was 0.73. Under the optimum conditions, copper was preconcentrated on the working electrode at -0.25 V（vs. SCE）. The anodic stripping voltammetric current increased linearly with copper concentration over the range of 0.01 -0. 325 μg·mL^-1. The correlation coefficient was 0. 9991, the recovery was 98.00%-100.56%, and the relative standard deviation was 2.27%-5.14%. The detection limit was 4.60×10^-3 μg·mL^-1 , and the interferences of Fe,Zn,Co and Ni with the determination were investigated. In the same way, the favourable concentration of the base solution of nickel contained 0.06 mol·L^-1 NH4OH-NH4Cl and pH value was 9.41. Under the optimum conditions, nickel was preconcentrated on the working electrode at -0.30 V （vs. SCE）. The anodic stripping vohammetric current increased linearly with nickel concentration over the range of 0. 5 - 6. 0 μg·mL^-1. The correlation coefficient was 0. 9996, the recovery was 98. 12% - 101. 73%, and the relative standard deviation was 3. 64% - 6. 21%. The detection limit was 0. 4422 μg·mL^-1, and the interferences of Al,Zn,Co and Cu with the determination were also investigated. This method has been used to determine the content of copper and nickel in ZSM- 5 zeoli catalyst with satisfactory results.

关 键 词：阳极溶出伏安法 铜 镍 ZSM-5催化剂 

分 类 号：O657.1[理学—分析化学]