基于离子液体基铂纳米流体电化学传感器的构建及其应用研究
发布时间：2019-05-14 12:11
【摘要】：纳米流体自被提出后广受关注,不同基质的纳米流体如水基、油基、液体石蜡基等不断被合成,并在生物医学、催化、制冷等方面得到不断应用。传统的纳米流体介质多为水、有机溶剂以及油,然而此类溶剂的热稳定性较差,挥发后对环境和人体健康造成影响。离子液体具有纳米流体介质所需的导热性和热稳定性,是名副其实的绿色溶剂,同时能够作为模板剂实现对无机纳米材料结构的控制,可以对纳米粒子进行表面修饰从而有效阻止纳米粒子团聚,这些特性为纳米流体的合成提供了新契机。本实验探索了在1-丁基-3-甲基咪唑四氟硼酸为介质,以离子液体中的聚乙烯基吡咯烷酮(PVP)为萃取剂,将水相中的[Pt Cl4]2-萃取到离子液体相中。在超声辅助条件下用硼氢化钠将离子液体相中的铂离子还原,制备了亲水性离子液体基铂纳米流体。同时对合成条件、纳米颗粒的形貌及稳定性进行了探讨。离子液体有宽电化学窗口和良好的导电性,纳米流体具有较好的导电性和高电催化活性,以离子液体为基质合成离子液体基纳米流体在电化学传感领域有着广阔的应用。本实验着重探讨了离子液体基铂纳米流体修饰电极构建电化学传感器用于尿酸、抗坏血酸和多巴胺的单组份和多组分测定,探索了离子液体基铂纳米流体在电分析化学领域的应用。本论文主要研究的内容和结果如下:1、[BMIm]BF4离子液体为介质,在1-丁基-3-甲基咪唑四氟硼酸/硫酸铵双水相体系中,聚乙烯吡咯烷酮(PVP)作萃取剂、稳定剂,在超声条件下制备1-丁基-3-甲基咪唑四氟硼酸铂纳米流体(Pt-[BMIm]BF4),同时用纳米粒度仪、透射电子显微镜、傅里叶红外光谱仪等对纳米流体进行表征。结果表明,制备的铂纳米流体中铂纳米颗粒平均粒度在31.2nm左右,且分布均匀、大小均一、稳定性好。PVP不仅阻止了纳米粒子间的团聚,还增强了铂纳米粒子的抗氧化性,获得了稳定的离子液体基铂纳米流。2、用离子液体基铂纳米流体(ILPtNFs)为修饰材料,制备电化学传感器,构建了测定多巴胺(DA)、尿酸(UA)、抗坏血酸(AA)的电化学传感器。采用循环伏安法研究了DA、UA、AA在该修饰电极上的电化学行为,以差示脉冲伏安法(DPV)建立了单独测定DA、UA、AA含量的方法。实验表明,分别在pH=3.0、pH=6.0和pH=6.0的磷酸缓冲溶液(PBS)中,ILPtNFs对AA、DA和UA具有明显的电催化作用。在最佳的实验条件下,DA氧化峰电流与其浓度在8.0×10-6-4.0×10-4 mol/l范围内呈良好的线性关系。UA氧化峰电流与其浓度在2.0×10-6-1.0×10-4 mol/l范围内呈良好的线性关系。AA氧化峰电流与其浓度在2.0×10-6-1.0×10-4 mol/l范围内呈良好的线性关系。将该方法分别用于盐酸多巴胺注射液中DA含量、人体尿液中UA含量、维生素C注射液中AA含量的测定,结果满意。3、滴涂法将ILPtNFs固定至玻碳电极表面制备电化学传感器,以差示脉冲伏安法(DPV)建立同时测定UA、DA和AA混合液的新方法。实验结果显示,ILPtNFs修饰电极能实现DA、UA和AA的良好分离。在实验优化条件下,当浓度在4.0×10-6 1.0×10-4 mol/l范围内时,分别改变UA、DA和AA的浓度,三者的峰电流与浓度呈良好的线性关系;同时改变UA、DA和AA的浓度,三者的峰电流与浓度呈良好的线性关系。该方法可用于实际样品中UA、DA和AA的定量检测,结果满意。
[Abstract]:The nano-fluid has been widely concerned since being put forward, and the nano-fluids of different substrates, such as water-based, oil-based, liquid paraffin, and the like, are continuously synthesized, and are continuously applied in the fields of biomedicine, catalysis, refrigeration and the like. The traditional nano-fluid medium is water, an organic solvent and oil, however, the thermal stability of such a solvent is poor, and the environment and the health of the human body are affected after volatilization. the ionic liquid has the thermal conductivity and the thermal stability required by the nano fluid medium, is a veritable green solvent, can be used as a template agent to control the structure of the inorganic nano material, These properties provide a new opportunity for the synthesis of nanofluids. In this experiment, the aqueous phase of[Pt _ 4] 2-in the aqueous phase was extracted into the ionic liquid phase with 1-butyl-3-methylcyclotetrafluoro-boric acid as the medium, and the polyethylene-based polyoxyalkanone (PVP) in the ionic liquid was used as the extractant. A hydrophilic ionic liquid-based platinum nano-fluid is prepared by reducing the platinum ions in the ionic liquid phase with sodium borohydride under the ultrasonic-assisted conditions. The morphology and stability of the nano-particles were also discussed. The ionic liquid has wide electrochemical window and good electrical conductivity, the nano fluid has good electrical conductivity and high electrocatalytic activity, and the ionic liquid is used as the matrix to synthesize the ionic liquid-based nano fluid and has wide application in the field of electrochemical sensing. The application of the ionic liquid-based platinum nano-fluid in the field of electroanalytical chemistry is discussed. The main contents and results of this thesis are as follows:1,[BMIm] BF4 ionic liquid is the medium, in the 1-butyl-3-medetomidine tetrafluoboric acid/ sulfuric acid aqueous two-phase system, the polyethylene and the alkanone (PVP) are used as the extractant and the stabilizer, 1-butyl-3-methyl-4-fluoroborate (Pt-[BMIm] BF4) was prepared under ultrasonic conditions, and the nano-fluid was characterized by a nano-particle size instrument, a transmission electron microscope, a Fourier transform infrared spectrometer, and the like. The results show that the average particle size of the platinum nanoparticles in the prepared platinum nano-fluid is about 31.2 nm, the distribution is uniform, the size is uniform, and the stability is good. The PVP not only prevents the agglomeration of the nano-particles, but also enhances the oxidation resistance of the platinum nano-particles, and obtains a stable ionic liquid-based platinum nano-flow.2, using the ionic liquid-based platinum nano-fluid (ILPtNFs) as a modified material, preparing an electrochemical sensor, and constructing a dopamine (DA), Electrochemical sensors for uric acid (UA), ascorbic acid (AA). The electrochemical behavior of DA, UA and AA on the modified electrode was studied by cyclic voltammetry, and the method of separately measuring the content of DA, UA and AA was established by differential pulse voltammetry (DPV). The results showed that ILPNFs had a significant electrocatalytic effect on AA, DA and UA in phosphate buffer (PBS) with pH = 3.0, pH = 6.0 and pH = 6.0, respectively. Under the best experimental conditions, the peak current of DA is in good linear relationship with its concentration in the range of 8.0-10-6-4.0-10-4mol/ l. The UA oxidation peak current has a good linear relationship with its concentration in the range of 2.0-10-6-1.0-10-4mol/ l. The peak current of AA is in a good linear relationship with its concentration in the range of 2.0-10-6-1.0-10-4mol/ l. The method is used for the determination of the content of DA in the dopamine injection of the hydrochloric acid, the content of the UA in the urine of the human body, the content of the AA in the vitamin C injection, and the result is satisfied. A new method for simultaneous determination of the mixture of UA, DA and AA was established by differential pulse voltammetry (DPV). The results show that the modified electrode of ILPNFs can realize the good separation of DA, UA and AA. 鍦ㄥ疄楠屼紭鍖栨潯浠朵笅,褰撴祿搴﹀湪4.0脳10-6 1.0脳10-4 mol/l鑼冨洿鍐呮椂,鍒嗗埆鏀瑰彉UA,DA鍜孉A鐨勬祿搴，
本文编号：2476705
[Abstract]:The nano-fluid has been widely concerned since being put forward, and the nano-fluids of different substrates, such as water-based, oil-based, liquid paraffin, and the like, are continuously synthesized, and are continuously applied in the fields of biomedicine, catalysis, refrigeration and the like. The traditional nano-fluid medium is water, an organic solvent and oil, however, the thermal stability of such a solvent is poor, and the environment and the health of the human body are affected after volatilization. the ionic liquid has the thermal conductivity and the thermal stability required by the nano fluid medium, is a veritable green solvent, can be used as a template agent to control the structure of the inorganic nano material, These properties provide a new opportunity for the synthesis of nanofluids. In this experiment, the aqueous phase of[Pt _ 4] 2-in the aqueous phase was extracted into the ionic liquid phase with 1-butyl-3-methylcyclotetrafluoro-boric acid as the medium, and the polyethylene-based polyoxyalkanone (PVP) in the ionic liquid was used as the extractant. A hydrophilic ionic liquid-based platinum nano-fluid is prepared by reducing the platinum ions in the ionic liquid phase with sodium borohydride under the ultrasonic-assisted conditions. The morphology and stability of the nano-particles were also discussed. The ionic liquid has wide electrochemical window and good electrical conductivity, the nano fluid has good electrical conductivity and high electrocatalytic activity, and the ionic liquid is used as the matrix to synthesize the ionic liquid-based nano fluid and has wide application in the field of electrochemical sensing. The application of the ionic liquid-based platinum nano-fluid in the field of electroanalytical chemistry is discussed. The main contents and results of this thesis are as follows:1,[BMIm] BF4 ionic liquid is the medium, in the 1-butyl-3-medetomidine tetrafluoboric acid/ sulfuric acid aqueous two-phase system, the polyethylene and the alkanone (PVP) are used as the extractant and the stabilizer, 1-butyl-3-methyl-4-fluoroborate (Pt-[BMIm] BF4) was prepared under ultrasonic conditions, and the nano-fluid was characterized by a nano-particle size instrument, a transmission electron microscope, a Fourier transform infrared spectrometer, and the like. The results show that the average particle size of the platinum nanoparticles in the prepared platinum nano-fluid is about 31.2 nm, the distribution is uniform, the size is uniform, and the stability is good. The PVP not only prevents the agglomeration of the nano-particles, but also enhances the oxidation resistance of the platinum nano-particles, and obtains a stable ionic liquid-based platinum nano-flow.2, using the ionic liquid-based platinum nano-fluid (ILPtNFs) as a modified material, preparing an electrochemical sensor, and constructing a dopamine (DA), Electrochemical sensors for uric acid (UA), ascorbic acid (AA). The electrochemical behavior of DA, UA and AA on the modified electrode was studied by cyclic voltammetry, and the method of separately measuring the content of DA, UA and AA was established by differential pulse voltammetry (DPV). The results showed that ILPNFs had a significant electrocatalytic effect on AA, DA and UA in phosphate buffer (PBS) with pH = 3.0, pH = 6.0 and pH = 6.0, respectively. Under the best experimental conditions, the peak current of DA is in good linear relationship with its concentration in the range of 8.0-10-6-4.0-10-4mol/ l. The UA oxidation peak current has a good linear relationship with its concentration in the range of 2.0-10-6-1.0-10-4mol/ l. The peak current of AA is in a good linear relationship with its concentration in the range of 2.0-10-6-1.0-10-4mol/ l. The method is used for the determination of the content of DA in the dopamine injection of the hydrochloric acid, the content of the UA in the urine of the human body, the content of the AA in the vitamin C injection, and the result is satisfied. A new method for simultaneous determination of the mixture of UA, DA and AA was established by differential pulse voltammetry (DPV). The results show that the modified electrode of ILPNFs can realize the good separation of DA, UA and AA. 鍦ㄥ疄楠屼紭鍖栨潯浠朵笅,褰撴祿搴﹀湪4.0脳10-6 1.0脳10-4 mol/l鑼冨洿鍐呮椂,鍒嗗埆鏀瑰彉UA,DA鍜孉A鐨勬祿搴，
本文编号：2476705
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