化学修饰电极的制备及其应用研究
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摘要
化学修饰电极是20世纪70年代中期发展起来的一门新兴的、也是当前最活跃的电化学和电分析化学的前沿领域,目前已应用于生命科学、环境科学、食品科学、分析科学以及材料科学等许多方面。聚合物修饰电极能够有目的地在电极表面固定所选择的化学功能团,赋予电极某种特定的性质,可以高选择地进行所期望的反应。修饰电极制备方法简单,电极使川寿命长,从而得以广泛使用。
本论文的采用化学或者电化学方法把特定官能团固定在电极表面,制备修饰电极,研究了该类修饰电极的电催化、吸附、富集等性能,并应用于Cu~(2+)离子和抗坏血酸的分析测定。
1.采用自组装和电化学循环伏安法,制得了L-半胱氨酸修饰金(L-Cys/Au)电极,探讨了L-Cys/Au电极的电化学特性,研究了该修饰电极表面Cu~(2+)离子的吸附伏安行为,在含铜离子的磷酸缓冲液(pH=6.86)中搅拌富集,铜离子吸附在L-Cys/Au电极表面.在一定浓度范围内Cu~(2+)离子浓度的对数值与Cu~(2+)离子的吸附还原峰电流(I_(pc))呈良好的线性关系,最低检测限可达2.0×10~(-10)mol/L,由此建立了一种灵敏的、选择性良好的检测痕量Cu~(2+)离子的电化学新方法。
2.通过电化学循环伏安法制备了L-谷氨酸/铁氰酸钾修饰玻碳电极,考察了Cu~(2+)离子在该修饰电极上的阳极溶出伏安行为,溶出峰电流(I_(pa))随Cu~(2+)离子浓度的增大而增大,并且在1.0×10~(-7)～1.0×10~(-3) mol/L浓度范围内,峰电流与Cu~(2+)离子浓度的对数存在良好的线性关系,建立了一种检测痕量铜离子的阳极溶出伏安新方法。
3.采用电聚合的方法制备了聚L-谷氨酸修饰玻碳电极,探讨了聚L-谷氨酸修饰玻碳电极的电化学行为,该修饰电极对抗坏血酸(AA)具有良好的电化学响应,并对实验测定条件进行了优化。实验结果表明,在pH=4.0的邻苯二甲酸氢钾缓冲溶液中,扫描电位为-0.2～1.0V范围内,抗坏血酸在聚L-谷氨酸修饰玻碳电极表面出现稳定的氧化峰。氧化峰的峰电流(I_(pa))与抗坏血酸的浓度在2.0×10~(-5)～2.0×10~(-3) mol/L范围内有良好的线性关系,最低检测限可达2.0×10~(-6)mol/L。该电极制备方便,有良好的稳定性和重现性。
Chemically modified electrode,developed in the middle of the 70s of 20~(th) century,is the most active frontier in electrochemistry and electroanalytical chemistry,which has been widely applied in life science,environmental science,food science,analytical science and material science.Some special function groups can be selected on purpose to be polymerized on the surface of electrode and thus the polymer film modified electrodes are endowed with some particular qualities to have highly selective reactions as expected.Therefore,with its simple preparation method and long working life, chemically modified electrode is widely used in many fields.
In this paper,the modified electrodes are prepared by some polymerizing special function groups onto the surface of electrode by chemical or electrochemical way.The properties of modified electrodes such as adsorbing capability and enrichment capability have been investigated.The modified electrodes have been successfully applied for the determination of Cu~(2+) ion and ascorbic acid.
1.The L-Cys/Au electrode was prepared by using self-assemble and electrochemical cyclic voltammetry.The electrochemical properties of L-Cys/Au electrode and the adsorption behavior of Cu~(2+) on the electrode surface were studied.Cu~(2+) ion was adsorbed on the surface of L-Cys/Au electrode when the PBS(pH=6.86) containing Cu~(2+) ion was stirred.Reduction peak current(I_(pc)) of Cu~(2+) ion has a good linear relationship with logarithm of Cu~(2+) concentration in a certain Cu~(2+) concentration range.The detection limit for Cu~(2+) was 2.0 x 10~(-10) mol/L.A new electrochemical method with highly sensitivity and selectivity for analyzing trace Cu~(2+) has been established.
2.The L-glutamic acid/Fe(CN)_6~(3-) modified glassy carbon electrode has been prepared by electrochemical cyclic voltammetry.The anticathode stripping behaviors of Cu~(2+) ion on the modified electrode was investigated.The stripping peak current(I_(pa)) increased with an increase in concentration of Cu~(2+) and was linear with logarithm of Cu~(2+) concentration in the range of 1.0×10~(-7)～1.0×10~(-3) mol/L.A new anticathode stripping voltammetry methode for the determination of trace Cu~(2+) was develpoed
3.The poly-L-glutamic acid modified glassy carbon electrode was prepared by electrochemical polymerization.The electrochemical behaviors of the modified electrode were investigated.The modified electrode had good electrochemical response for ascorbic acid.The experimental conditions for the determination of ascorbic acid were optimized and the results showed that ascorbic acid in pH 4.0 buffer solution had steady oxidation peak on the surface of the poly-L-glutamic acid modified glassy carbon electrode in the scanning potential range of -0.2～1.0 V.The oxidation peak current(I_(pa)) has a good linear relationship with the concentration of ascorbic acid in the range of 2.0 x 10~(-5)～2.0×10~(-3) mol/L with the detection limit of 2.0×10~(-6) mol/L.The preparation of this electrode with good stability and repeatability is convenient.
本论文的采用化学或者电化学方法把特定官能团固定在电极表面,制备修饰电极,研究了该类修饰电极的电催化、吸附、富集等性能,并应用于Cu~(2+)离子和抗坏血酸的分析测定。
1.采用自组装和电化学循环伏安法,制得了L-半胱氨酸修饰金(L-Cys/Au)电极,探讨了L-Cys/Au电极的电化学特性,研究了该修饰电极表面Cu~(2+)离子的吸附伏安行为,在含铜离子的磷酸缓冲液(pH=6.86)中搅拌富集,铜离子吸附在L-Cys/Au电极表面.在一定浓度范围内Cu~(2+)离子浓度的对数值与Cu~(2+)离子的吸附还原峰电流(I_(pc))呈良好的线性关系,最低检测限可达2.0×10~(-10)mol/L,由此建立了一种灵敏的、选择性良好的检测痕量Cu~(2+)离子的电化学新方法。
2.通过电化学循环伏安法制备了L-谷氨酸/铁氰酸钾修饰玻碳电极,考察了Cu~(2+)离子在该修饰电极上的阳极溶出伏安行为,溶出峰电流(I_(pa))随Cu~(2+)离子浓度的增大而增大,并且在1.0×10~(-7)～1.0×10~(-3) mol/L浓度范围内,峰电流与Cu~(2+)离子浓度的对数存在良好的线性关系,建立了一种检测痕量铜离子的阳极溶出伏安新方法。
3.采用电聚合的方法制备了聚L-谷氨酸修饰玻碳电极,探讨了聚L-谷氨酸修饰玻碳电极的电化学行为,该修饰电极对抗坏血酸(AA)具有良好的电化学响应,并对实验测定条件进行了优化。实验结果表明,在pH=4.0的邻苯二甲酸氢钾缓冲溶液中,扫描电位为-0.2～1.0V范围内,抗坏血酸在聚L-谷氨酸修饰玻碳电极表面出现稳定的氧化峰。氧化峰的峰电流(I_(pa))与抗坏血酸的浓度在2.0×10~(-5)～2.0×10~(-3) mol/L范围内有良好的线性关系,最低检测限可达2.0×10~(-6)mol/L。该电极制备方便,有良好的稳定性和重现性。
Chemically modified electrode,developed in the middle of the 70s of 20~(th) century,is the most active frontier in electrochemistry and electroanalytical chemistry,which has been widely applied in life science,environmental science,food science,analytical science and material science.Some special function groups can be selected on purpose to be polymerized on the surface of electrode and thus the polymer film modified electrodes are endowed with some particular qualities to have highly selective reactions as expected.Therefore,with its simple preparation method and long working life, chemically modified electrode is widely used in many fields.
In this paper,the modified electrodes are prepared by some polymerizing special function groups onto the surface of electrode by chemical or electrochemical way.The properties of modified electrodes such as adsorbing capability and enrichment capability have been investigated.The modified electrodes have been successfully applied for the determination of Cu~(2+) ion and ascorbic acid.
1.The L-Cys/Au electrode was prepared by using self-assemble and electrochemical cyclic voltammetry.The electrochemical properties of L-Cys/Au electrode and the adsorption behavior of Cu~(2+) on the electrode surface were studied.Cu~(2+) ion was adsorbed on the surface of L-Cys/Au electrode when the PBS(pH=6.86) containing Cu~(2+) ion was stirred.Reduction peak current(I_(pc)) of Cu~(2+) ion has a good linear relationship with logarithm of Cu~(2+) concentration in a certain Cu~(2+) concentration range.The detection limit for Cu~(2+) was 2.0 x 10~(-10) mol/L.A new electrochemical method with highly sensitivity and selectivity for analyzing trace Cu~(2+) has been established.
2.The L-glutamic acid/Fe(CN)_6~(3-) modified glassy carbon electrode has been prepared by electrochemical cyclic voltammetry.The anticathode stripping behaviors of Cu~(2+) ion on the modified electrode was investigated.The stripping peak current(I_(pa)) increased with an increase in concentration of Cu~(2+) and was linear with logarithm of Cu~(2+) concentration in the range of 1.0×10~(-7)～1.0×10~(-3) mol/L.A new anticathode stripping voltammetry methode for the determination of trace Cu~(2+) was develpoed
3.The poly-L-glutamic acid modified glassy carbon electrode was prepared by electrochemical polymerization.The electrochemical behaviors of the modified electrode were investigated.The modified electrode had good electrochemical response for ascorbic acid.The experimental conditions for the determination of ascorbic acid were optimized and the results showed that ascorbic acid in pH 4.0 buffer solution had steady oxidation peak on the surface of the poly-L-glutamic acid modified glassy carbon electrode in the scanning potential range of -0.2～1.0 V.The oxidation peak current(I_(pa)) has a good linear relationship with the concentration of ascorbic acid in the range of 2.0 x 10~(-5)～2.0×10~(-3) mol/L with the detection limit of 2.0×10~(-6) mol/L.The preparation of this electrode with good stability and repeatability is convenient.
引文
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