TiO2光催化降解4-氯苯酚过程中的电分析监测

采用循环伏安法和紫外光谱法对有机物的光催化降解进行机理研究和在线监测.以标准光催化剂DegussaP25在紫外光照射下催化降解4-氯苯酚,发现在降解过程中至少有两对氧化还原中间产物对苯二酚-苯醌和羟基氢醌-羟基苯醌.由4-氯苯酚及中间产物的电极响应,可以观测到它们在光催化降解过程中的含量变化,从而对整个过程实现在线监测,并由此全面了解光催化反应机理.从不同反应时间后测得的紫外光谱可以看到,苯环特征峰逐渐消失.这表明4-氯苯酚的苯环逐渐被打开,直至被彻底降解.     

二氧化钛多孔薄膜对含氯苯酚的电助光催化降解

用涂膜法制备了具有多孔微结构的二氧化钛薄电极,以制得的电极为工作电极,建立了三电极的电助光催化体系。选择含氟苯酚（４－氯苯酚,２,４,６－三氯苯酚）作为降解对象,进行光催化研究。实验结果表明,外加电极偏压可抑制光生电子－空穴的复合,提高二氧化钛的光催化效率;光强越强,降解速度越快。     

水中硝基酚的纳米TiO2光催化降解

以主波长254nm的紫外灯作为光源,研究了锐钛型纳米TiO2对邻硝基苯酚、2,4－二硝基苯酚的光催化降解行为,并与普通TiO2作了对比;结果表明,纳米TiO2表现出很高的光催化活性,催化降解过程符合一级动力学规律。     

纳米TiO2光催化降解苯酚的动力学研究

以１２５Ｗ高压汞灯为光源,以ＴｉＯ２为催化剂,对不同初始浓度的苯酚水溶液进行了光催化降解实验。同时,考察了不同溶液ｐＨ值时的光催化行为。根据实验结果,提出了与文献报道不同的ＴｉＯ２光催化降解苯酚的零级反应动力学模型。     

玻璃负载TiO2膜光催化降解2,4-二氯苯酚

玻璃负载TiO2膜光催化降解2;4-二氯苯酚     

纳米TiO2光催化降解聚乙二醇反应

纳米TiO2光催化降解聚乙二醇反应;纳米二氧化钛; 光催化; 聚乙二醇     

TiO2薄膜光催化降解4-(2-吡啶偶氮)间苯二酚的研究

为了探索有机物４－（２－吡啶偶氮）间苯二酚（ＰＡＲ）,在固定光催化剂上的降解行为,采用溶胶一凝胶法,在玻璃表面制得均匀透明的纳米ＴｉＯ２薄膜,并以其作光催化剂,在２５４ｎｍ紫外光照射下,进行ＰＡＲ水溶液的光催化降解研究。研究了ＰＡＲ光催化降解率与溶液ｐＨ值、ＰＡＲ初始浓度、助催化剂（Ｈ２Ｏ２）浓度和不同光照条件的变化关系,得出了ＴｉＯ２薄膜的光催化降解ＰＡＲ的有利条件。     

活性炭负载TiO2光催化降解1-萘胺

活性炭负载TiO2光催化降解1-萘胺;炭载TiO2光催化剂;萘胺;光催化降解     

光催化降解苯酚污染物的电化学监测——推荐一个分析化学综合实验

针对目前高校开展的分析化学实验教学内容单一,侧重常规分析方法以及仪器基本原理介绍等问题,将综合性实验教学项目引入到教学中,能够增强学生独立探索、主动思考和分析问题的能力。本文设计了基于纳米TiO2光催化剂催化降解苯酚的综合性实验方案,涉及光催化降解和电化学监测的原理,以及光催化降解和电化学装置的搭建等。     

一步低温法制备可见光响应的棕色纳米TiO2及其光催化性能

光催化作为一种具有前景的技术,被广泛运用于有机物降解、废水处理、空气净化、抗菌、太阳能电池等领域.在众多的光催化材料中,纳米TiO2因具有性质稳定、耐腐蚀、廉价和无毒等优点而受到广泛关注.但纳米TiO2禁带宽度较大(3.2 eV)、只对紫外光有响应及电子-空穴对易复合等特性限制了它的应用.因此,提高纳米TiO2的可见光响应一直是研究的热点.本文发展了一种在低温下制备棕色纳米TiO2的改良溶胶-凝胶法.该法以钛酸四丁酯为钛源,无水乙醇为溶剂,形成溶胶后无需陈化和高温高压,在简单温和的条件下即可制备出棕色纳米TiO2.比较了低温干燥和高温焙烧两种处理方法,结果表明,随着制备温度的升高,样品的粒子尺寸增大,比表面积减小,颜色从白色转变为棕色,在更高的温度又变浅.样品的可见光吸收在180℃时达到最大,随后减弱.在优化温度180℃下制备的TiO2-180℃纳米粒子不仅具有较小的粒径(5.0 nm),较大的比表面积(213.45 m2/g),且在整个紫外-可见光区都具有较强的吸收,其禁带宽度低至1.84 eV.X-射线光电子能谱结果表明,TiO2粒子表面的–OH/H2O含量随制备温度升高而先增加后下降.Raman光谱中Eg峰的移动和变宽表明TiO2晶格可能存在缺陷或氧空位,而TiO2-180℃纳米粒子的电子顺磁共振图谱的g值在2.003左右,对应氧空位中的未成对电子,验证了以上推测.其中TiO2-180℃纳米粒子呈现为最强的EPR信号,表明其晶格内存在最高浓度的氧空位,这是其具有强可见光吸收的原因.光催化实验结果表明,在可见光照射下,TiO2-180℃可高效降解亚甲基蓝(MB).当C(MB)=10 mg/L,pH=4,催化剂添加量为0.07 g时,TiO2-180℃催化剂的光催化活性达到最佳,光照1 h后MB降解率达到99.33%,反应速率常数(0.08287 mg/(L·min))约为同条件下P25(0.01342 mg/(L·min))的6倍.同时,TiO2-180℃催化剂在不同单色光下的光催化活性与它对单色光的光响应大致相符.循环降解实验证明TiO2-180℃催化剂具有很好的稳定性.光猝灭实验表明,·OH在光催化降解过程占主导作用,而TiO2-180℃样品表面含有较多的–OH,有利于·OH的产生,乃至光催化反应.研究表明,晶格内高浓度的氧空位导致的强可见光响应,得益于低温制备条件而保留了大量–OH/H2O的纳米粒子表面以及更大的比表面积,共同促成了TiO2-180℃优越的光催化活性.所制备的棕色纳米TiO2经过进一步修饰后有望运用于实际应用中.     

Electrooxidation of Formamidine Disulfide Simultaneously Investigated by On-Line High Performance Liquid Chromatography and Cyclic Voltammetry

The electro-oxidation of formamidine disulfide, an important sulfur-containing compound, was simultaneously investigated with on-line high-performance liquid chromatography and cyclic voltammetry. Using a home-made microporous sampler located at the electrode interface, the solution on the electrode surface was in situ sampled and analyzed. The electrochemical scanning was synchronously performed, which allowed the electro-oxidation products to be detected at a given potential. The main products on the surface of platinum electrode were found to be thiourea, formamidine sulfinic acid, cyanamide, and elemental sulfur. Forced convection arising from the sampling played an important role in the electrochemical oxidation. The extraction of electrode surface solution promoted the renewal of reactant and its intermediates, which induced the change of cyclic voltammetry curve. The forced convection also contributed to the redox peak current of the species on the cyclic voltammetry curves through the change of concentration of reactant and its intermediates. This technique can help to explore the reaction mechanism of complex electrochemical reactions.     

Monitoring of Polymerized Triglycerides in Deep-Frying Oil by On-Line GPC-FTIR Spectrometry Using the Science Based Calibration Multivariate Approach

On-line gel permeation chromatography Fourier transform infrared (GPC-FTIR) is proposed as detection technique for the determination of the total polymer triacylglyceride (PTG) content in olive oil as an alternative to other conventional detectors such as the evaporative light scattering detector (ELSD) or the refraction index detector (RID). FTIR detection allowed confirmation additionally to quantification of the analytes via their characteristic infrared spectra. For the extraction of chromatograms, a multivariate method called science based calibration (SBC) was used. The SBC method employed a reference spectrum of triacylglycerides (TG) extracted from the injection of a fresh olive oil sample and data obtained from a blank injection as ‘noise’ matrix, to estimate a regression vector subsequently used to predict the relative concentration of the analyte during the GPC run. Results found evidenced that the use of SBC improved the selectivity, sensitivity and repeatability of the GPC-FTIR measurements as compared to the ‘classical’ approach based on the measurement of the spectral area in a defined spectral range. The developed method provided a limit of detection for PTGs of 0.19 mg mL^?1, which corresponds to a 0.65% w/w for an oil sample mass of 300 mg.     

Discrimination of Beers by Cyclic Voltammetry Using a Single Carbon Screen-printed Electrode

A fast, simple and costless methodology without sample pre-treatment is proposed for the discrimination of beers. It is based on cyclic voltammetry (CV) using commercial carbon screen-printed electrodes (SPCE) and includes a correction of the signals measured with different SPCE units. Data are submitted to partial least squares discriminant analysis (PLS−DA) and support vector machine discriminant analysis (SVM−DA), which allow a reasonable classification of the beers. Also, CV data from beers can be used to predict their alcoholic degree by partial least squares (PLS) and artificial neural networks (ANN). In general, non-linear methods provide better results than linear ones.     

Monitoring of Methyldopa by Fast Fourier Transform Continuous Cyclic Voltammetry at Gold Microelectrode

A continuous cyclic voltammetric study of methyldopa at gold micro electrode was carried out. The drug in phosphate buffer (pH 2.0) is adsorpted at 400 mV, giving rise to change in the current of well-defined oxidation peak of gold in the flow injection system. The proposed detection method has some of advantages, the greatest one of which are as follows: first, it is no more necessary to remove oxygen from the analyte solution and second, this is a very fast and appropriate technique for determination of the drug compound in a wide variety of chromatographic analysis methods. Signal-to-noise ratio has significantly increased by application of discrete Fast Fourier transform (FFT) method, background subtraction and two-dimensional integration of the electrode response over a selected potential range and time window. Also in this work some parameters such as sweep rate, eluent pH, and accumulation time and potential were optimized. The linear concentration range was of 1.0×10－7—1.0×10－11 mol•L－1 (r＝0.9975) with a limit of detection and quantitation 0.004 nmol•L－1 and 0.03 nmol•L－1, respectively. The method has the requisite accuracy, sensitivity, precision and selectivity to assay methyldopa in tablets. The influences of pH of eluent, accumulation potential, sweep rate, and accumulation time on the determination of the methyldopa were considered.     

循环伏安法研究超分子有机凝胶中二茂铁的扩散

4,4′-二(硬脂酰胺基)-二苯甲烷(BSAPM)在LiClO4/碳酸丙烯酯(PC)中能形成超分子有机凝胶。用循环伏安法研究了包埋在凝胶中的二茂铁的氧化还原行为。结果表明,有机凝胶内的二茂铁仍具有氧化还原活性,其氧化还原行为是受扩散控制的单电子可逆转移过程。与溶液相比,最低化凝胶浓度下凝胶中二茂铁和二茂铁离子的扩散系数分别从5.62×10-6cm2/s和6.47×10-6cm2/s下降为3.32×10-6cm2/s和4.41×10-6cm2/s,且随凝胶因子浓度的增加,凝胶中二茂铁和二茂铁离子的扩散系数降低。     

血液中葡萄糖含量的伏安法测定

在磷酸盐生理缓冲溶液中，葡萄糖的浓度在一定范围内与循环伏法（ＣＶ）的峰电流线性关系，利用这一关系，进行了多份血液样品中葡萄糖含量的测定，并与例行的“葡萄糖氧化酶－氧化物酶比色法”（ＧＣＤ）测定的结果作比较，发现测定结果是满意的。     

循环伏安法测定磺胺嘧啶

循环伏安法测定磺胺嘧啶;磺胺嘧啶;测定;多壁碳纳米管;修饰玻碳电极;循环伏安法     

Exploring the Bioelectrochemical Characteristics of Activated Sludge Using Cyclic Voltammetry

Due to the potential interest, bioelectrochemical responses of activated sludge using the three-electrode system are tested. From the cyclic voltammograms, the oxidation current output is increasing due to incubation time increase, whereas 5, 25 and 39.33 μA are obtained after 3, 72 and 96 h, respectively. Changing the working electrode from glassy carbon to carbon paste led to the increase in the electrochemical signal from 0.3 to be 3.72 μA. On the other hand, the use of the lipophilic redox mediator (2,6-dichlorophenolindophenol (DCIP)) amplified the oxidation current to reach 19.9 μA instead of 2.1 μA. Based on these findings, the mixed microbial community of the activated sludge is exploited as a catalyst for the bio-oxidation of the degradable organic substrates, while DCIP is used as a mobile electron carrier from the intracellular matrix of the metabolically active cells to the carbon paste electrode which served as the final electron acceptor. Therefore, the extracellular electron transfer from the formed active biofilm at the electrode surface is assisted by the existence of DCIP.