碳纳米管修饰电极用于染料—环糊精超分子体系的研究
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摘要
第一章:简要概述了修饰电极、碳纳米管、环糊精的基本内容,综述了近年来染料与环糊精相互作用的研究进展。
第二章:采用循环伏安法研究了活性艳橙K-7R在玻碳电极上的电化学行为。在0.2mol·L~(-1)(pH 7.0)Na_2HPO_4-KH_2PO_4缓冲液中,活性艳橙K-7R在-100 mV(vs.SCE)处有一对稳定、灵敏的氧化还原峰,其峰电流与浓度在1.0×10~(-7)～1.0×10~(-5)mol·L~(-1)范围内呈良好的线性关系,检测限为4.0×10~(-8)mol·L~(-1),RSD为2.61%。用“直线法”测定了活性艳橙K-7R与几种不同环糊精的包结比和包结常数,比较了包结能力,探讨了包结位点及影响包结能力大小的因素。
第三章:制备了MWNTs/Nafion修饰玻碳电极,详细研究了灿烂甲酚紫(BCV)在电极上的电化学行为。发现MWNTs/nafion复合膜可以较好的电催化BCV,BCV在修饰电极上发生了2电子2质子氧化还原反应。采用差示脉冲伏安法研究了BCV与γ-CD、HP-γ-CD的相互作用,计算了包结比和包结常数。此外,用分光光度法和~1HNMR法进一步证实了包结物的形成。结果表明,BCV可以在γ-CD空腔内形成H-聚集体。γ-CD和HP-γ-CD与该染料的二聚体均形成1:1的包结物,包结常数分别为2650 L·mol~(-1)和8040 L·mol~(-1),修饰环糊精的包结能力大于母体环糊精,说明体积匹配是包结物形成的决定性因素。
第四章:考察了甲基紫(MV)、乙基紫(EV)在MWNTs/Nafion修饰玻碳电极上的电化学行为。MV和EV在修饰电极上均发生了2电子2质子氧化还原反应,MV呈现出较EV强的电子转移能力;在溶液中,MV的扩散系数也略高于EV。采用差示脉冲伏安法研究了MV、EV与β-CD及其衍生物的相互作用,计算了包结比和包结常数。实验结果表明,各种环糊精对EV的包结能力均大于对MV的包结能力;MV、EV与各种环糊精的包结能力顺序均为:CM-β-CD＞HP-β-CD＞TM-β-CD＞DM-β-CD＞β-CD。包结常数的大小说明EV的分子尺寸更适于被β-CD包结。修饰环糊精的包结能力大于母体环糊精,说明体积匹配和疏水作用是包结物形成的决定性因素。而CM-β-CD显示出的强的包结能力则进一步证实静电作用对包合物的形成具有一定的贡献。
第五章:蓝色盐VB在酸性介质中易于聚合成二聚体或高聚体,在MWNTs/Nafion修饰玻碳电极表面发生2电子2质子的氧化还原反应。与环糊精形成包结物后,VB的扩散系数增加,导致峰电流增大,同时也阻碍了重氮盐分子的聚合。HP-β-CD、β-CD、HP-α-CD及α-CD与蓝色盐VB均形成1:1的包结物,不同的环糊精与VB的包结能力强弱次序为:HP-β-CD＞β-CD＞HP-α-CD＞α-CD,而γ-CD空腔太大不适合包合VB。
Chapter 1:The fundamental contents of modified electrodes,carbon nanotubes and cyclodextrins were briefly introduced.The research progress of the interaction between dyes and cyclodextrins(CDs) in recent years was summarized in details.
Chapter 2:The electrochemical behavior of Reactive Brilliant Orange K-7R at glassy carbon electrode was studied by cyclic voltammetry method.The result showed that Reactive Brilliant Orange K-7R had a stable and sensitive oxidation-reduction peak at about-100mV in 0.2mol·L~(-1) Na_2HPO_4-KH_2PO_4 (pH 7.0) buffer solution.The peak current is proportional to the concentration in the range of 1.0×10~(-7)～1.0×10~(-5)mol·L~(-1).The limit of detection is 4.0×10~(-8) mol·L~(-1) and RSD is 2.61%.The corresponding inclusion ratio and inclusion constant were determined by "straight line method".The inclusion ability between the dye and different kinds of cyclodextrins was compared. Furthermore,the possible inclusion mechanism was proposed.
Chapter 3:MWNTs/Nafion modified GCE was fabricated and used to study the electrochemical behavior of Brilliant Cresyl violet(BCV).It was found that MWNTs/Nafion composite membrane was able to electrocatalyze BCV, and the redox of BCV involved two electrons and two protons.The inclusion interaction between BCV withγ-CD and HP-γ-CD were studied based on the differential pulse voltammetry(DPV) method.The inclusion ratio and inclusion constants were calculated.The formation inclusion complexes of BCV withγ-CD were further confirmed by UV-Vis and ~1HNMR spectrophotometry.The result showed that two BCV molecules could form H-aggregation in the cavity ofγ-CD.γ-CD and HP-γ-CD could form 1:1 inclusion complex with the dimmer of BCV,and the inclusion constants were 2650 L·mol~(-1) and 8040 L·mol~(-1),respectively.The inclusive ability of modifiedγ-CD was stronger than the nativeγ-CD,which further indicated the major factor was size matching in the progress of forming inclusior complex.
Chapter 4:The electrochemical behavior and the reaction mechanism of methyl violet(MV) and ethyl violet(EV) on the MWNTs/Nafion modified GCE were investigated in detail.The redox of MV and EV involved two electrons and two protons,and electron transfer ability and diffusion coefficient of MV were stronger than those of EV.The inclusion interaction of MV and EV withβ-CD and its derivatives were studied by DPV method, respectively.The inclusion ratios and inclusion constants were all calculated by "straight line method".The experimental showed thatβ-CD and its derivatives also presented stronger inclusion ability towards EV.The inclusion ability order of CDs is CM-β-CD＞HP-β-CD＞TM-β-CD＞DM-β-CD＞β-CD.The inclusion constants suggested that the molecular size of EV is more suitable for the cavity ofβ-CD.Inclusion capacity of modified CDs was greater than that of the native CDs,indicating the major factors affecting inclusive ability are size matching and hydrophobicity.However, CM-β-CD showed stronger inclusive ability,suggesting the charge interaction between CDs and guest had addtional contribution.
Chapter 5:In acid solution,Fast Blue Salt VB was easy to aggregate into dimer or high polymer,and exhibited two electrons and two protons redox process on the modified electrode.The diffusion coefficient of VB increased with the formation of inclusion complexes with CDs,and lead to the increase of the peak current.In addition,the formation of inclusion complexes prohibited the polymerization of diazonium salt molecules.VB could form 1:1 inclusion complexes with HP-β-CD,β-CD,HP-α-CD andα-CD with the inclusion ability order of HP-β-CD＞β-CD＞HP-α-CD＞α-CD,andγ-CD was not suitable for inclusion due to the larger cavity.
第二章:采用循环伏安法研究了活性艳橙K-7R在玻碳电极上的电化学行为。在0.2mol·L~(-1)(pH 7.0)Na_2HPO_4-KH_2PO_4缓冲液中,活性艳橙K-7R在-100 mV(vs.SCE)处有一对稳定、灵敏的氧化还原峰,其峰电流与浓度在1.0×10~(-7)～1.0×10~(-5)mol·L~(-1)范围内呈良好的线性关系,检测限为4.0×10~(-8)mol·L~(-1),RSD为2.61%。用“直线法”测定了活性艳橙K-7R与几种不同环糊精的包结比和包结常数,比较了包结能力,探讨了包结位点及影响包结能力大小的因素。
第三章:制备了MWNTs/Nafion修饰玻碳电极,详细研究了灿烂甲酚紫(BCV)在电极上的电化学行为。发现MWNTs/nafion复合膜可以较好的电催化BCV,BCV在修饰电极上发生了2电子2质子氧化还原反应。采用差示脉冲伏安法研究了BCV与γ-CD、HP-γ-CD的相互作用,计算了包结比和包结常数。此外,用分光光度法和~1HNMR法进一步证实了包结物的形成。结果表明,BCV可以在γ-CD空腔内形成H-聚集体。γ-CD和HP-γ-CD与该染料的二聚体均形成1:1的包结物,包结常数分别为2650 L·mol~(-1)和8040 L·mol~(-1),修饰环糊精的包结能力大于母体环糊精,说明体积匹配是包结物形成的决定性因素。
第四章:考察了甲基紫(MV)、乙基紫(EV)在MWNTs/Nafion修饰玻碳电极上的电化学行为。MV和EV在修饰电极上均发生了2电子2质子氧化还原反应,MV呈现出较EV强的电子转移能力;在溶液中,MV的扩散系数也略高于EV。采用差示脉冲伏安法研究了MV、EV与β-CD及其衍生物的相互作用,计算了包结比和包结常数。实验结果表明,各种环糊精对EV的包结能力均大于对MV的包结能力;MV、EV与各种环糊精的包结能力顺序均为:CM-β-CD＞HP-β-CD＞TM-β-CD＞DM-β-CD＞β-CD。包结常数的大小说明EV的分子尺寸更适于被β-CD包结。修饰环糊精的包结能力大于母体环糊精,说明体积匹配和疏水作用是包结物形成的决定性因素。而CM-β-CD显示出的强的包结能力则进一步证实静电作用对包合物的形成具有一定的贡献。
第五章:蓝色盐VB在酸性介质中易于聚合成二聚体或高聚体,在MWNTs/Nafion修饰玻碳电极表面发生2电子2质子的氧化还原反应。与环糊精形成包结物后,VB的扩散系数增加,导致峰电流增大,同时也阻碍了重氮盐分子的聚合。HP-β-CD、β-CD、HP-α-CD及α-CD与蓝色盐VB均形成1:1的包结物,不同的环糊精与VB的包结能力强弱次序为:HP-β-CD＞β-CD＞HP-α-CD＞α-CD,而γ-CD空腔太大不适合包合VB。
Chapter 1:The fundamental contents of modified electrodes,carbon nanotubes and cyclodextrins were briefly introduced.The research progress of the interaction between dyes and cyclodextrins(CDs) in recent years was summarized in details.
Chapter 2:The electrochemical behavior of Reactive Brilliant Orange K-7R at glassy carbon electrode was studied by cyclic voltammetry method.The result showed that Reactive Brilliant Orange K-7R had a stable and sensitive oxidation-reduction peak at about-100mV in 0.2mol·L~(-1) Na_2HPO_4-KH_2PO_4 (pH 7.0) buffer solution.The peak current is proportional to the concentration in the range of 1.0×10~(-7)～1.0×10~(-5)mol·L~(-1).The limit of detection is 4.0×10~(-8) mol·L~(-1) and RSD is 2.61%.The corresponding inclusion ratio and inclusion constant were determined by "straight line method".The inclusion ability between the dye and different kinds of cyclodextrins was compared. Furthermore,the possible inclusion mechanism was proposed.
Chapter 3:MWNTs/Nafion modified GCE was fabricated and used to study the electrochemical behavior of Brilliant Cresyl violet(BCV).It was found that MWNTs/Nafion composite membrane was able to electrocatalyze BCV, and the redox of BCV involved two electrons and two protons.The inclusion interaction between BCV withγ-CD and HP-γ-CD were studied based on the differential pulse voltammetry(DPV) method.The inclusion ratio and inclusion constants were calculated.The formation inclusion complexes of BCV withγ-CD were further confirmed by UV-Vis and ~1HNMR spectrophotometry.The result showed that two BCV molecules could form H-aggregation in the cavity ofγ-CD.γ-CD and HP-γ-CD could form 1:1 inclusion complex with the dimmer of BCV,and the inclusion constants were 2650 L·mol~(-1) and 8040 L·mol~(-1),respectively.The inclusive ability of modifiedγ-CD was stronger than the nativeγ-CD,which further indicated the major factor was size matching in the progress of forming inclusior complex.
Chapter 4:The electrochemical behavior and the reaction mechanism of methyl violet(MV) and ethyl violet(EV) on the MWNTs/Nafion modified GCE were investigated in detail.The redox of MV and EV involved two electrons and two protons,and electron transfer ability and diffusion coefficient of MV were stronger than those of EV.The inclusion interaction of MV and EV withβ-CD and its derivatives were studied by DPV method, respectively.The inclusion ratios and inclusion constants were all calculated by "straight line method".The experimental showed thatβ-CD and its derivatives also presented stronger inclusion ability towards EV.The inclusion ability order of CDs is CM-β-CD＞HP-β-CD＞TM-β-CD＞DM-β-CD＞β-CD.The inclusion constants suggested that the molecular size of EV is more suitable for the cavity ofβ-CD.Inclusion capacity of modified CDs was greater than that of the native CDs,indicating the major factors affecting inclusive ability are size matching and hydrophobicity.However, CM-β-CD showed stronger inclusive ability,suggesting the charge interaction between CDs and guest had addtional contribution.
Chapter 5:In acid solution,Fast Blue Salt VB was easy to aggregate into dimer or high polymer,and exhibited two electrons and two protons redox process on the modified electrode.The diffusion coefficient of VB increased with the formation of inclusion complexes with CDs,and lead to the increase of the peak current.In addition,the formation of inclusion complexes prohibited the polymerization of diazonium salt molecules.VB could form 1:1 inclusion complexes with HP-β-CD,β-CD,HP-α-CD andα-CD with the inclusion ability order of HP-β-CD＞β-CD＞HP-α-CD＞α-CD,andγ-CD was not suitable for inclusion due to the larger cavity.
引文
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