基于石墨烯电化学传感器的构建及对偶氮类色素的应用

发布时间：2018-02-26 18:29

本文关键词： 石墨烯电化学传感器偶氮类色素　出处：《郑州大学》2015年硕士论文　论文类型：学位论文

【摘要】：石墨烯是一种独特的sp2杂化的单层碳原子结构的新型二维材料,自2004年第一次出现就引起了人们的广泛关注。石墨烯由于具备优异的机械强度、大的特殊的比表面积以及高超的导电性等优点,因此被大量的应用于超级电容器、电池以及传感器等领域。石墨烯层与层之间存在较强的范德华力,使得石墨烯容易团聚,难以分散在常用的溶剂中,因此需要通过有效的功能化方法来改善石墨烯的分散性,发挥其优异的性能。纳米金属及氧化物材料具有电子转移速率快、催化效率高等特点,因此在光学、电化学和催化等领域表现出优越的应用前景。纳米金属及氧化物材料具备尺寸较小、比表面积较大和活性位点较多等催化剂的基本要求,在有机反应中是一类重要的催化剂。无论是贵金属Pt、Pd还是非贵金属金属Co、Ni以及金属氧化物WO3等,它们的催化活性都普遍较高,在催化剂领域应用比较广泛。食用色素是人们生活中常用的添加剂之一,过量的使用会对人体健康产生危害作用,特别是经过有机反应合成的偶氮类色素。日落黄、柠檬黄、诱惑红和苋菜红等色素是国家允许食用的偶氮类色素,并且国家规定了其在食品中的最大添加量。食品中色素的含量超标会对人体健康产生毒副作用,因此对色素的使用进行有效的检测和控制十分必要。本论文基于阳离子表面活性剂CTAB和PDDA功能化的石墨烯负载多种纳米金属及氧化物材料形成的复合材料,构建了灵敏检测四种偶氮类合成色素的电化学传感器。通过TEM、紫外光谱、红外光谱、XRD、EIS等多种方法对合成材料及修饰电极进行表征,采用CV、DPV等方法研究了修饰电极对偶氮类色素的高效灵敏的电催化性能,最后应用于实际样品分析,得到良好的结果。1.CTAB-Gr-Pt/GCE修饰电极的制备及对日落黄的测定本实验通过静电自组装的方式合成CTAB-Gr-Pt复合物,建立了新型灵敏的CTAB-Gr-Pt/GCE电化学传感器。由于石墨烯和纳米Pt的大的比表面积和电催化作用,因此CTAB-Gr-Pt复合物能够提高日落黄的电化学信号。通过TEM、紫外光谱法、红外光谱法、EIS等方法对复合材料及修饰电极进行表征,采用CV和DPV方法研究了日落黄在CTAB-Gr-Pt/GCE修饰电极上的电化学行为。在最优条件下,日落黄的线性范围是0.08-10.0μmol/L,检出限是4.2 nmol/L。该方法灵敏度较高,可以用于饮料中日落黄的测定并得到满意的回收结果。2.PDDA-Gr-Pd/GCE修饰电极的制备及对日落黄和柠檬黄的同时测定本实验基于PDDA-Gr-Pd复合物构建了同时测定日落黄和柠檬黄的新型的电化学传感器。PDDA作为一种阳离子表面活性剂可以把纳米Pd吸附到石墨烯的表面。由于石墨烯和纳米Pd的大表面积和导电性的协同作用,PDDA-Gr-Pd复合物对日落黄和柠檬黄的电化学信号表现出良好的选择性和灵敏性。通过TEM、紫外光谱法、XRD、EIS等方法对复合材料及修饰电极进行表征,采用CV和DPV方法研究了日落黄和柠檬黄在PDDA-Gr-Pd/GCE修饰电极上的电化学行为。在最优条件下,日落黄和柠檬黄的线性范围分别为0.01-10.0μmol/L和0.01-8.0μmol/L,检出限分别为2.0 nmol/L和5.0 nmol/L。此方法简单灵敏,能够同时测定饮料中日落黄和柠檬黄的含量并得到满意的结果。3.PDDA-Gr-Ni/GCE修饰电极的制备及对诱惑红的测定本实验基于PDDA-Gr-Ni复合物构建了灵敏测定诱惑红的电化学传感器。通过TEM、紫外光谱法、XRD、EIS等方法对复合材料及修饰电极进行表征,采用CV和DPV方法研究了诱惑红在PDDA-Gr-Ni/GCE修饰电极上的电化学行为。实验发现,PDDA-Gr-Ni复合物良好的电催化作用能够提高诱惑红的电化学响应信号。在最优条件下,诱惑红的线性范围为0.05-10.0μmol/L,检出限为8.0nmol/L。此方法简单灵敏,成功的用于饮料中诱惑红的测定,并得到满意的回收结果。4.PDDA-Gr-WO3/GCE修饰电极的制备及对苋菜红的测定本实验成功制备了基于PDDA-Gr-WO3复合物测定苋菜红的新型灵敏的电化学传感器。通过TEM、紫外光谱法、EIS等方法对复合材料及修饰电极进行表征,采用CV和DPV方法研究了苋菜红在PDDA-Gr-WO3/GCE修饰电极上的电化学行为。实验结果表明,在最优条件下,苋菜红的线性范围为0.01-10.0μmol/L,检出限为6.0 nmol/L。此方法成功用于饮料中苋菜红的测定,并得到满意的回收结果。
[Abstract]:Graphene is a novel two-dimensional material monolayer carbon atom structure of a unique SP2 hybrid, the first time since 2004 has aroused extensive attention. The graphene with excellent mechanical strength, large specific surface area and the advantages of high conductivity, because this is widely used in super capacitors, batteries and field sensors. The existence of strong Fan Dehua forces between the graphene layers and makes graphene easy to agglomerate, difficult to disperse in common solvents, so we need to improve the dispersion of graphene by functional methods effectively, its excellent performance. And the nano metal oxide material with electronic transfer rate, high catalytic efficiency, therefore in the optical, electrochemical and catalytic fields showed a good application prospect. The nano metal and oxide materials with smaller size, specific surface area The basic requirements of larger and more active sites of the catalyst in organic reactions, is a kind of important catalyst. Both the noble metal Pt, Pd or non noble metal Co, Ni and WO3 metal oxides and their catalytic activity are generally higher than in the field of application, catalyst widely edible pigment is one of the most commonly used. The additive of people's life, excessive use will cause harm to human health, especially after azo pigment organic reaction. Sunset yellow, lemon yellow, amaranth and Allura red pigment is a kind of azo pigment state allows the consumption, and the provisions of the state on the food in the largest amount. The content of pigment in food exceed the standard will produce toxic side effects on human health, therefore the use of pigment effective detection and control is very necessary. This paper based on cationic surfactant CTAB and PDDA function The load of graphene composite material to form a variety of nano metal and oxide materials, construct four kinds of electrochemical sensors for sensitive detection of azo pigment by TEM, UV, IR, XRD, EIS and other methods of characterization, synthetic materials and the modified electrodes by CV, DPV and other methods of modification dual electrode nitrogen pigment high electrocatalytic performance sensitive, finally applied to the analysis of actual samples, obtained good results.1.CTAB-Gr-Pt/GCE modified electrode preparation and the experiment by electrostatic self-assembly on the determination of sunset yellow synthetic CTAB-Gr-Pt complex, the establishment of a new sensitive electrochemical CTAB-Gr-Pt/GCE sensor. The graphene and nano Pt large surface area and electrocatalysis, so CTAB-Gr-Pt complexes can improve the electrochemical signal of sunset yellow by TEM, UV spectroscopy, infrared light Spectrum method, EIS method was used to characterize the composite material and modified electrode, studied the electrochemical behavior of sunset yellow in CTAB-Gr-Pt/GCE modified glassy carbon electrode. Using CV and DPV method under the optimal conditions, the linear range is 0.08-10.0, sunset yellow mol/L, the detection limit is 4.2 nmol/L. the method has high sensitivity, and can be used for the determination of beverage sunset yellow was recovered with satisfactory results of.2.PDDA-Gr-Pd/GCE modified electrode preparation and at the same time of sunset yellow and lemon yellow determination of the experimental PDDA-Gr-Pd complex was constructed based on Simultaneous Determination of sunset yellow and lemon yellow novel electrochemical sensor.PDDA as a cationic surfactant can be adsorbed onto the surface of nano Pd because of graphene. The synergistic effect of graphene and nano Pd with large surface area and conductivity, electrochemical signals of PDDA-Gr-Pd complex on sunset yellow and lemon yellow showed good The selectivity and sensitivity by TEM, UV, XRD, EIS and other methods were used to characterize the composite materials and the modified electrode of sunset yellow and lemon yellow on the electrochemical behavior of PDDA-Gr-Pd/GCE modified glassy carbon electrode. Using CV and DPV method under the optimal conditions, the linear range of sunset yellow lemon Huang Hening were 0.01-10.0. Mol/L and 0.01-8.0 mol/L, the detection limits were 2 nmol/L and 5 nmol/L., this method is simple and sensitive, can simultaneously determine the content in drink lemon yellow and sunset yellow and obtain satisfactory results of.3.PDDA-Gr-Ni/GCE modified electrode preparation and determination of Allura red in this experiment, the PDDA-Gr-Ni complex is constructed based on electrochemical sensor of red sensitive determination of temptation by TEM, UV, XRD, EIS and other methods were used to characterize the composite material and modified electrode, were studied on PDDA-Gr-Ni/GCE modified by Allura red CV and DPV method The electrochemical behavior of the electrode. It was found that the electrocatalytic activity of PDDA-Gr-Ni composite good can improve the electrochemical response of Allura red signal. Under the optimal conditions, the linear range is 0.05-10.0 ~ mol/L red temptation, the detection limit is 8.0nmol/L. this method is simple and sensitive, successfully applied to the determination of Allura red drink, and get the results with the.4.PDDA-Gr-WO3/GCE modified electrode preparation and determination of amaranth in this experiment was successfully prepared a new sensitive electrochemical sensor of PDDA-Gr-WO3 complexes based on the determination of amaranth. By TEM, UV, EIS and other methods were used to characterize the composite material and modified electrode of amaranth on PDDA-Gr-WO3/GCE modified electrode electrochemical behavior on using CV and DPV methods. The experimental results show that under the optimal conditions, the linear range of amaranth is 0.01-10.0 mol/L, the detection limit was 6 nmol/ L. this method has been successfully used for the determination of amaranth in beverage, and the satisfactory recovery results are obtained.

【学位授予单位】：郑州大学
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：TQ127.11;TP212.2

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