膜流动电位测试中Ag-AgCl电极的制备及稳定性研究
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摘要
膜的动电特性研究中,往往采用流动电位方法。该方法中,Ag-Ag Cl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-Ag Cl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-Ag Cl电极稳定性的影响。得到Ag-Ag Cl电极的最优制备参数为:电流密度3.0m A/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AgAg Cl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 AgAg Cl electrode was the key element to affect the test accuracy. The factors which impact the Ag-Ag Cl 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-Ag Cl electrode was as follows: the current density is 3. 0m A/cm2,chlorination time is 50 min,hydrochloric acid concentration is 0. 1mol·L-1,the baking temperature 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-Ag Cl electrode prepared under optimal conditions was test. The electrode having a strong stability,the electrode potential shift amounts are less than 0. 10 mv and0. 2mv in 24 h 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 formula,R2>0. 99,with good linearity and repeatability to meet the requirement of membrane streaming potential test.
In the research of membrane electric properties,often using streaming potential method. In this method,the quality of AgAg Cl electrode was the key element to affect the test accuracy. The factors which impact the Ag-Ag Cl 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-Ag Cl electrode was as follows: the current density is 3. 0m A/cm2,chlorination time is 50 min,hydrochloric acid concentration is 0. 1mol·L-1,the baking temperature 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-Ag Cl electrode prepared under optimal conditions was test. The electrode having a strong stability,the electrode potential shift amounts are less than 0. 10 mv and0. 2mv in 24 h 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 formula,R2>0. 99,with good linearity and repeatability to meet the requirement of membrane streaming potential test.
引文
[1]谢辉玲,叶红齐,曾坚贤.流动电位和通量法表征中空纤维超滤膜的污染程度及清洗效果[J].水处理技术,2006,(5):36-38.
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[8]钟惠萍,冯珍鸽,王力.(NH4)42[Mo132O372(CH3COO)30(H2O)72]膜修饰电极的构筑和电化学性质的研究[J].化学研究与应用,2010,(3):384-386.
[9]张彦成,杨庆,常青.聚偏氟乙烯中空纤维膜的低温等离子体改性及动电特性研究[J].水处理技术,2011,(3):57-61.
[10]何为,薛卫东,唐斌.优化试验设计方法及数据处理分析[M].北京:化学工业出版社,2012,35-41.
[11]邱轶兵.实验设计与数据处理[M].合肥:中国科学技术大学出版社,2008,101-150.
[12]Wang M,Wu L G,Zheng X C,et al.Surface modification of phenolphthalein poly(ether sulfone)、ultrafiltration membranes by blending with acrylonitrile based copolymer containing ionic groups for imparting surface electrical properties[J].J Colloid Interf Sci,2006,300(1):286-292.
[13]王建,王晓琳.膜动电现象的研究进展[J].水处理技术.2002,(6):311-315,372.
[2]PontiéM,Durand-Bourlier L,Lemordant D,et al.Control fouling and cleaning procedures of UF membranes by a streaming potential method[J].Sep Purif Technolo,1998,14(1):1-11.
[3]邱运仁,缪畅,叶红齐.聚砜中空纤维超滤膜的流动电位研究[J].膜科学与技术,2009,(6):75-80.
[4]谢声洛.离子选择电极分析技术[M].北京:化学工业出版社,1985,117-120.
[5]杨渝,李龙,刘红伟,等.全固态裸露式Ag/Ag Cl参比电极的研制及应用[J].化学传感器,2011,(3):45-48.
[6]卫云鸽,曹全喜,雷梦碧.全固体Ag/Ag Cl电极的制备工艺研究[J].功能材料,2010,(S3):441-444.
[7]王颉.试验设计与SPSS应用[M].北京:化学工业出版社,2007,86-115.
[8]钟惠萍,冯珍鸽,王力.(NH4)42[Mo132O372(CH3COO)30(H2O)72]膜修饰电极的构筑和电化学性质的研究[J].化学研究与应用,2010,(3):384-386.
[9]张彦成,杨庆,常青.聚偏氟乙烯中空纤维膜的低温等离子体改性及动电特性研究[J].水处理技术,2011,(3):57-61.
[10]何为,薛卫东,唐斌.优化试验设计方法及数据处理分析[M].北京:化学工业出版社,2012,35-41.
[11]邱轶兵.实验设计与数据处理[M].合肥:中国科学技术大学出版社,2008,101-150.
[12]Wang M,Wu L G,Zheng X C,et al.Surface modification of phenolphthalein poly(ether sulfone)、ultrafiltration membranes by blending with acrylonitrile based copolymer containing ionic groups for imparting surface electrical properties[J].J Colloid Interf Sci,2006,300(1):286-292.
[13]王建,王晓琳.膜动电现象的研究进展[J].水处理技术.2002,(6):311-315,372.