Synthesis of 5-[(2-hydroxynaphthalen-1-yl)diazenyl]isophthalic acid and its application to electrocatalytic oxidation and determination of adrenaline,paracetamol, and tryptophan

In this study,Au nanoparticles/poly 5-[(2-hydroxynaphthalen-l-yl)diazenyl]isophthalic acid film modified glassy carbon electrode(AuNPs/poly(NDI)/GCE) has shown excellent electrocatalytic activity toward the oxidation of adrenaline(ADR),paracetamol(PAC),and tryptophan(Trp).The bare glassy carbon electrode(GCE) fails to separate the oxidation peak potentials of these molecules,while the poly(NDI) film modified electrode can resolve them.Electrochemical impedance spectroscopy(EIS)indicates that the charge transfer resistance of the bare electrode decreases as 5-[(2-hydroxynaphthalen-l-yl)diazenyl]isophthalic acid is electropolymerized on the bare electrode.Furthermore,EIS exhibits enhancement of electron transfer kinetics between analytes and the electrode after electrodeposition of Au nanoparticles.Differential pulse voltammetry results show that the electrocatalytic current increases linearly in the ranges of 0.01-680.0 μmol L~1 for ADR,0.05-498.0 μmol L~1 for PAC,and 3.0-632.0 μmol L~1 for Trp;with detection limits(S/N = 3) of 0.009 μmol L~1,0.005 μmol L~1,and 0.09 μmol L~1 for ADR,PAC,and Trp,respectively.The proposed method has been successfully applied for simultaneous determination of ADR,PAC,and Trp in biological samples.     

Characterization of Sixteenth to Nineteenth Century Ottoman Silk Brocades by Scanning Electron Microscopy–Energy Dispersive X-Ray Spectroscopy and High-Performance Liquid Chromatography

Historical textiles in the Topkap? Museum, which are called silk kaftans and brocades by art historians from the sixteenth and nineteenth were characterized by scanning electron microscopy–energy dispersive X-ray spectroscopy (SEM–EDX) and high-performance liquid chromatography with diode array detection for identification of metal threads and dyestuffs. In the most Ottoman textiles, metal threads, especially belonging to the sultans, were used as the gold gild. Although the chemical composition of the samples on the surface may easily be obtained by SEM–EDX, the thickness of the thin gold layer on metal threads cannot be obtained directly. Hence, the goal of this project is to describe whether metal threads are gilded or not and to measure coating thickness. A new method was developed for measuring the thickness of gold layer, and the modeling was reformed. The SEM–EDX results were interpreted in accordance with the theoretical models. The coating thickness of metal threads was subsequently measured in ancient textiles. The thickness, depth, and valuable metal composition in the threads of the artistic objects were obtained by this approach. Dye analysis was used to characterize the presence of indigotin, carminic acid, ellagic acid, and luteolin in the historical textiles.     

新式夹心型光透薄层光谱电化学电解池

本文设计了一种新式夹心型光透薄层紫外-可见光谱电化学池。该池采用铂网工作电极,两侧平行放置铂片为对极置于同一石英窗口夹层中,同时以聚四氟乙烯隔离膜作为边际限制器,结合池内小孔道设置内参比点进行精确的电位控制,具有理想的光谱电化学响应。利用循环伏安、循环电位-吸收、恒电位现场光谱、双电位跃-计时电量、双电位跃-计时吸收等技术,对铁氰化钾在氯化钾溶液中的行为进行了表征。     

Effect of enzyme concentration on the dynamic behavior of a membrane-bound enzyme system

The dynamic behavior of the reaction-diffusion system, composed of glucose oxidase (EC 1.1.3.4) immobilized at a uniform concentration in a membrane, used as a glucose electrode is represented by a diffusion equation with a nonlinear reaction-term in one-dimensional space. The mathematical model is analyzed by computer simulation, that is, numerical integration of the equation under various initial and boundary conditions, to examine the effect of enzyme concentration on the response characteristics (responsiveness and linearity in response) of the electrode. The analysis of the responses of the system to stepwise changes in the boundary value (glucose concentration in simple solution) infers that the enzyme concentration governs the patterns of the spatial distributions of the substrates (glucose and dissolved oxygen) in steady states and transient responses. It is also revealed that the response characteristics of the electrode are optimized with concentration of immobilized enzyme and that the system establishes the steady states at the same spatial distributions of the substrates, regardless of the boundary value. The diffusion of the substrates and the oxygen concentration also have significant effects on the response characteristics of the electrode.     

金在碳糊电极上的静电吸附及溶出伏安测定

阳极溶出伏安法测定金具有灵敏度高,操作简便等优点,但共存金属往往干扰测定,影响该方法的应用。为减少干扰,已有阴极溶出伏安法的报道。 作者曾采用修饰了三烷基叔胺的碳糊电极,通过开路萃取富集和介质交换,测定矿样中的金,并且发现,碳糊电极本身能在正电位下直接富集微量金,在阴极溶出伏安法中显示了     

(4,4′,4″,4″′-四硝基)·酞菁合钴(Ⅱ)化学修饰电极对抗坏血酸的电催化氧化

合成了一种钴的酞菁配合物,以玻碳为基体、用化学吸附法制备了它的化学修饰电极。用CV法研究了该化学修饰电极对抗坏血酸氧化的电催化作用。结果表明,该化学修饰电极对抗坏血酸的氧化有一定的电催化作用,且电催化活性的稳定性高,抗坏血酸的电催化氧化峰电流和其浓度之间有良好的线性关系。     

铜电极表面的电致发光法现场测试

采用电致发光等方法, 初步探讨了铜电极在0.25 mol·L~(-1)Na_2S_2O_8+1.25 mol·L~(-1)NaOH溶液中的电致发光特性及其相关性能, 给出了电致发光法现场测试铜电极表面性质的初步结果。     

金属蒸气合成法制备燃料电池电极催化剂Ⅰ.Ag_n/C电极的制备及性质

金属蒸气合成法(MVS)已用于新材料的制备。我们曾报道用此法制备负载型金属催化剂。本文报道用MVS法制备的Ag_n/C燃料电池电极的结构与催化性能。     

KCl-LiCl-H2O体系热力学性质的研究

用K-ISE、Li-ISE和Cl-ISE测定了25 ℃时体系中KCl、LiCl的平均活度系数, 溶液的离子强度从0.1～4.0 mol·kg~(-1), 组成范围从纯的KCl到纯的LiCl。将Pitzer方程应用于测定结果, 用多元线性回归方法求出了Pitzer参数。     

集成微管路离子选择电极功能块研究

本文对微型管状离子选择电极在流动条件下的电化学特征进行了研究,并设计了新的集成微管路离子选择以电极功能块。用此微型装置测定了土壤、血清、水和药物中的K~+、Na~+、pH、Cl~-、F~-、阿托品、东茛菪碱,并和各种标准方法作了比较,获得满意分析结果。