膜的动电特性研究中,往往采用流动电位方法。该方法中,Ag-AgCl测试电极的质量是影响测试准确性的关键要素。本文采用正交试验设计和方差分析,着重考察电解法制备Ag-AgCl电极过程中,电流强度( I)、氯化时间(t)、电解质溶液浓度(CHCl)、电极来源(n)、烘烤温度(T)、活化电极溶液浓度(CKCl)等因素对Ag-AgCl电极稳定性的影响。得到Ag-AgCl电极的最优制备参数为:电流密度3.0mA/cm2,氯化时间50min,盐酸浓度0.1mol·L-1,烘烤温度120℃,活化电极溶液(KCl)浓度0.001mol·L-1;最显著影响因素为电极来源,显著影响因素为氯化时间和烘烤温度。对最优条件组合下制备的Ag-AgCl电极,进行了稳定性实验,结果表明:制备的电极具有较好的稳定性,24h内电极电位漂移量小于0.10mv,7天内电极电位漂移量小于0.2mv;在聚偏氟乙烯中空纤维超滤膜流动电位测试中,流动电位与流动压差具有良好的线性和可重复性,回归曲线R2〉0.99,变化规律符合Helmholtz-Smoluehowski公式,可以较好满足膜的流动电位测试要求。
In the research of membrane electric properties,often using streaming potential method. In this method,the quality of Ag-AgCl electrode was the key element to affect the test accuracy. The factors which impact the Ag-AgCl electrode quality and stability in the electrolytic preparation process,including the current intensity(I),chlorinated time(t),the concentration of the electrolyte solution(CHCl),the source of electrode(n),the baking temperature(T),the concentration of activation the electrode solution ( CKCl ) ,were studied by means of orthogonal test and variance analysis. The optimal parameters of Ag-AgCl electrode was as fol-lows:the current density is 3. 0mA/cm2 ,chlorination time is 50min,hydrochloric acid concentration is 0. 1mol·L-1 ,the baking tem-perature is 120℃,storing electrolyte concentration is 0. 001 mol·L-1;the most significant affecting factor is the source of electrode,the significant affecting factors are baking temperature and chlorination time. The stability of the Ag-AgCl electrode prepared under optimal conditions was test. The electrode having a strong stability,the electrode potential shift amounts are less than 0. 10mv and 0. 2mv in 24h and in 7 days respectively. The prepared electrode was used in polyvinylidene fluoride hollow fiber ultrafiltration membrane streaming potential test,the potential change with pressure is in line with the variation of Helmholtz-Smoluehowski formu-la,R2〉0. 99,with good linearity and repeatability to meet the requirement of membrane streaming potential test.