纳米材料修饰电极及在环境分析中的应用研究
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摘要
纳米材料具有的小尺寸效应、表面与界面效应、量子尺寸效应和宏观量子隧道等效应及由此产生的一系列独特的物理、化学性质使其已成为当前科技领域的研究热点,在纳米电子学、纳米化学、传感器、环境检测、医药、生物技术等诸多领域已有较多的应用。分子印迹技术是指为得到在空间结构和结合位点上与某一模板分子完全匹配、且对模板分子具有特异识别能力的新型聚合物的实验制备技术。分子印迹聚合物敏感材料与生物敏感材料如酶、抗体等相比,具有抗恶劣环境、稳定性高和使用寿命长等优点,因此在分析分离,特别是固相萃取、膜分离技术、异构体分离、传感器等领域获得广泛研究。目前,运用纳米材料作为化学修饰电极的修饰材料是化学修饰电极新的发展方向。本论文主要将贵金属纳米粒子、纳米管等纳米材料应用于构建电化学传感器。将纳米金属和碳纳米管制备成复合材料,利用它们具有的协同作用以期得到较高的电催化活性;利用氨基对金溶胶的强烈亲和作用在氨基硅烷修饰电极上自组装一层纳米金,以期利用纳米金的高催化活性提高电化学传感器的灵敏度;同时利用了高选择性的分子印迹技术,制备自组装分子印迹膜电极,提高电化学传感器的选择性。本论文的具体研究内容包括:
1.以碳纳米管(CNTs)和氯铂酸为原料制备铂微粒/碳纳米管修饰电极(Pt/CNTs/GCE)。铂微粒采用循环伏安法电化学沉积制备。以该修饰电极作为甲醛的电化学传感器,用循环伏安法(CV)和线性扫描伏安法(LSV)研究了甲醛在该电极上的电化学行为,优化了实验条件,在此基础上建立了一种测定甲醛的伏安分析方法。
2.以碳纳米管(CNTs)和氯金酸为原料制备纳米金/碳纳米管修饰电极(Au /CNTs/GCE)。纳米金采用循环伏安法电化学沉积制备。用循环伏安法和线性扫描伏安法研究了甲基对硫磷在该电极上的电化学行为。FE-SEM和XRD技术表征了修饰膜的特性。考察了电解质溶液的pH值及富集时间、纳米金的负载量等因素对于对硫磷的还原峰电流的影响。
3.以含有氨基的硅烷,如N-[3-(三甲氧硅基)丙基]-乙二胺及3-氨丙基-三乙氧基硅烷与金溶胶通过自组装制备亚硝酸盐的电化学传感器。用循环伏安法、微分脉冲伏安法(DPV)及微分脉冲安培法(DPA)研究了亚硝酸盐在该电极上的电化学行为。
4.以对硫磷为模板分子,四丁基高氯酸铵为支持电解质,邻氨基硫酚为聚合物单体,用电聚合的方法在金电极上制备自组装邻氨基硫酚分子印迹膜。用印迹膜修饰电极和非印迹膜修饰电极对一系列与对硫磷相近的化合物如甲基对硫磷、对氧磷、辛硫磷和氧乐果、硝基苯及邻、间、对硝基苯酚进行检测。
5.通过电聚合在玻碳电极上将磷钨杂多酸掺杂在聚吡咯中,制备了磷钨杂多酸/聚吡咯修饰玻碳电极(PW12/PPY/GCE)。用Nafion作为离子选择性渗透膜排除抗坏血酸根、尿酸根和硝酸根等阴离子的干扰。用循环伏安法研究了Nafion/PW12/PPY/GC的电化学行为,并用微分脉冲伏安法和微分脉冲安培法研究了NO在该修饰电极上的电化学行为。
The small size effect, the surface and interface effect, the quantum size effect and the macroscopic quantum tunnel effect of nanometer materials results in series of interesting physical and chemical properties, which have become hotspots in scientific and technological fields in recent year. The nano-materials have been applied in many fields including nanoelectronics, nanochemistry, sensors, environmental monitoring, medicine, biotechnology and so on. Molecular imprinting is a method for making selective binding sites in synthetic polymers by using a molecular template. After the removal of the template, the remaining polymer gives rise to“memory sites”that are sterically and chemically complementary to the imprint species. Compared to the natural entities such as antibodies and enzymes, the artificially generated molecular recognition materials possess the virtue of anti-harsh environment, high stability and long use life which made them is useful for analytical separations, in particular in solid-phase extraction, membrane separation technique, separation of isomers and sensors.
At present, the application of nano-materials as new chemically modified materials is a new trend in the field of chemically modified electrodes. In this paper, precious metals nanoparticles, carbon nanotubes were applied to composite electrochemical sensors. Nanoparticles/nanotubes composite possess interesting synergistic properties which can enhance the catalysis activity of the modified electrodes. With the high affinity of the–NH2 groups towards gold surface, gold nanoparticles can be self-assembled on the electrode and acted as excellent catalyst. Due to the high selectivity of molecular imprinting technolygy, the self-assembled imprinting film modified electrodes were constructed. In detail, the thesis including such study as follows:
1. Platinum particles were electrochemically deposited on glassy carbon electrodes (GCE) modified with carbon nanotubes. The chemically modified glassy carbon electrodes with platinum particles and carbon nunotubes (Pt/CNTs/GCE) were used as formaldehyde sensors. Electrochemica1 behaviors of formaldehyde at Pt/CNTs/GCE were investigated by cyclic voltammetry (CV) and linear scan voltammetry (LSV). Experimental conditions were optimized, and a voltammetric method for determining formaldehyde was developed.
2. Gold nanoparticles were electrochemically deposited on glassy carbon electrodes modified with carbon nanotubes (Au/CNTs/GCE). Electrochemica1 behaviours of methyl-parathion at Au/CNTs/GCE were investigated by cyclic voltammetry and linear scan voltammetry. Field emission scanning electron microscope (FE-SEM) and X-ray diffraction (XRD) techniques were used for characterization of the composite. The effect of pH, accumulation time and amount of the deposited gold microparticles on the reduction peak current of methyl-parathion at the Au/MWCNTs/GCE were investigated.
3. The modified sensors were fabricated by N-[3-(trimethoxysilyl) propyl]-ethylene diamine (TSPED) or (3-aminopropyl)-trimethoxysilane on glass carbon electrodes. Colloidal gold particles were modified by self-assembling onto the amine groups of the sol-gel. Electrochemica1 behaviours of nitrite on sol-gol and gold nanoparticles modified glassy carbon electeodes (AuNPs/TSPED/GCE) and AuNPs/ATS/GCE were investigated by differential pulse voltammetry (DPV) and differential pulse amperometry (DPA).
4. Cyclic voltammetry was employed in the process of electropolymerization on gold electrode. Parathion was used as template molecule; tetrabutyl ammonium perchlorate was used as supporting electrolyte and o-aminothiophenol as polymer monomer. Parathion imprinted and nonimprinted polymer films were exposed to a series of closely related compounds and the sensor exhibited good selectivity and sensitivity to parathion.
5. A polypyrrole (PPY) doped by phosphotungstic heteropolyacid (PW12) and Nafion (Nf) doubly layer modified glassy carbon electrode (Nf/PW12/PPY/GCE) was prepared. The Nafion layer modified on the surface of electrocatalyst could effectively eliminate the interferences from common species anion in biological samples such as ascorbate, urate and nitrite. The electrochemical behaviours of nitric oxide at the Nf/PW12/PPY/GCE were investigated by cyclic voltammetry.
1.以碳纳米管(CNTs)和氯铂酸为原料制备铂微粒/碳纳米管修饰电极(Pt/CNTs/GCE)。铂微粒采用循环伏安法电化学沉积制备。以该修饰电极作为甲醛的电化学传感器,用循环伏安法(CV)和线性扫描伏安法(LSV)研究了甲醛在该电极上的电化学行为,优化了实验条件,在此基础上建立了一种测定甲醛的伏安分析方法。
2.以碳纳米管(CNTs)和氯金酸为原料制备纳米金/碳纳米管修饰电极(Au /CNTs/GCE)。纳米金采用循环伏安法电化学沉积制备。用循环伏安法和线性扫描伏安法研究了甲基对硫磷在该电极上的电化学行为。FE-SEM和XRD技术表征了修饰膜的特性。考察了电解质溶液的pH值及富集时间、纳米金的负载量等因素对于对硫磷的还原峰电流的影响。
3.以含有氨基的硅烷,如N-[3-(三甲氧硅基)丙基]-乙二胺及3-氨丙基-三乙氧基硅烷与金溶胶通过自组装制备亚硝酸盐的电化学传感器。用循环伏安法、微分脉冲伏安法(DPV)及微分脉冲安培法(DPA)研究了亚硝酸盐在该电极上的电化学行为。
4.以对硫磷为模板分子,四丁基高氯酸铵为支持电解质,邻氨基硫酚为聚合物单体,用电聚合的方法在金电极上制备自组装邻氨基硫酚分子印迹膜。用印迹膜修饰电极和非印迹膜修饰电极对一系列与对硫磷相近的化合物如甲基对硫磷、对氧磷、辛硫磷和氧乐果、硝基苯及邻、间、对硝基苯酚进行检测。
5.通过电聚合在玻碳电极上将磷钨杂多酸掺杂在聚吡咯中,制备了磷钨杂多酸/聚吡咯修饰玻碳电极(PW12/PPY/GCE)。用Nafion作为离子选择性渗透膜排除抗坏血酸根、尿酸根和硝酸根等阴离子的干扰。用循环伏安法研究了Nafion/PW12/PPY/GC的电化学行为,并用微分脉冲伏安法和微分脉冲安培法研究了NO在该修饰电极上的电化学行为。
The small size effect, the surface and interface effect, the quantum size effect and the macroscopic quantum tunnel effect of nanometer materials results in series of interesting physical and chemical properties, which have become hotspots in scientific and technological fields in recent year. The nano-materials have been applied in many fields including nanoelectronics, nanochemistry, sensors, environmental monitoring, medicine, biotechnology and so on. Molecular imprinting is a method for making selective binding sites in synthetic polymers by using a molecular template. After the removal of the template, the remaining polymer gives rise to“memory sites”that are sterically and chemically complementary to the imprint species. Compared to the natural entities such as antibodies and enzymes, the artificially generated molecular recognition materials possess the virtue of anti-harsh environment, high stability and long use life which made them is useful for analytical separations, in particular in solid-phase extraction, membrane separation technique, separation of isomers and sensors.
At present, the application of nano-materials as new chemically modified materials is a new trend in the field of chemically modified electrodes. In this paper, precious metals nanoparticles, carbon nanotubes were applied to composite electrochemical sensors. Nanoparticles/nanotubes composite possess interesting synergistic properties which can enhance the catalysis activity of the modified electrodes. With the high affinity of the–NH2 groups towards gold surface, gold nanoparticles can be self-assembled on the electrode and acted as excellent catalyst. Due to the high selectivity of molecular imprinting technolygy, the self-assembled imprinting film modified electrodes were constructed. In detail, the thesis including such study as follows:
1. Platinum particles were electrochemically deposited on glassy carbon electrodes (GCE) modified with carbon nanotubes. The chemically modified glassy carbon electrodes with platinum particles and carbon nunotubes (Pt/CNTs/GCE) were used as formaldehyde sensors. Electrochemica1 behaviors of formaldehyde at Pt/CNTs/GCE were investigated by cyclic voltammetry (CV) and linear scan voltammetry (LSV). Experimental conditions were optimized, and a voltammetric method for determining formaldehyde was developed.
2. Gold nanoparticles were electrochemically deposited on glassy carbon electrodes modified with carbon nanotubes (Au/CNTs/GCE). Electrochemica1 behaviours of methyl-parathion at Au/CNTs/GCE were investigated by cyclic voltammetry and linear scan voltammetry. Field emission scanning electron microscope (FE-SEM) and X-ray diffraction (XRD) techniques were used for characterization of the composite. The effect of pH, accumulation time and amount of the deposited gold microparticles on the reduction peak current of methyl-parathion at the Au/MWCNTs/GCE were investigated.
3. The modified sensors were fabricated by N-[3-(trimethoxysilyl) propyl]-ethylene diamine (TSPED) or (3-aminopropyl)-trimethoxysilane on glass carbon electrodes. Colloidal gold particles were modified by self-assembling onto the amine groups of the sol-gel. Electrochemica1 behaviours of nitrite on sol-gol and gold nanoparticles modified glassy carbon electeodes (AuNPs/TSPED/GCE) and AuNPs/ATS/GCE were investigated by differential pulse voltammetry (DPV) and differential pulse amperometry (DPA).
4. Cyclic voltammetry was employed in the process of electropolymerization on gold electrode. Parathion was used as template molecule; tetrabutyl ammonium perchlorate was used as supporting electrolyte and o-aminothiophenol as polymer monomer. Parathion imprinted and nonimprinted polymer films were exposed to a series of closely related compounds and the sensor exhibited good selectivity and sensitivity to parathion.
5. A polypyrrole (PPY) doped by phosphotungstic heteropolyacid (PW12) and Nafion (Nf) doubly layer modified glassy carbon electrode (Nf/PW12/PPY/GCE) was prepared. The Nafion layer modified on the surface of electrocatalyst could effectively eliminate the interferences from common species anion in biological samples such as ascorbate, urate and nitrite. The electrochemical behaviours of nitric oxide at the Nf/PW12/PPY/GCE were investigated by cyclic voltammetry.
引文
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