[Co(1,10-phen)(H_2O)(VO_3)_2]的水热合成、结构及电化学性质

采用水热方法并以邻菲啉为模板剂合成了一种过渡金属配合物连接的无机-有机层状结构的多金属钒酸盐Co(1,10-phen)(H2O)(VO3)2,该化合物经过X-射线单晶衍射、元素分析、红外光谱表征和热失重分析,并用循环伏安法研究了标题化合物的电化学性质.     

Review on recent and advanced applications of monoliths and related porous polymer gels in micro-fluidic devices

This review critically summarises recent novel and advanced achievements in the application of monolithic materials and related porous polymer gels in micro-fluidic devices appearing within the literature over the period of the last 5 years (2005-2010). The range of monolithic materials has developed rapidly over the past decade, with a diverse and highly versatile class of materials now available, with each exhibiting distinct porosities, pore sizes, and a wide variety of surface functionalities. A major advantage of these materials is their ease of preparation in micro-fluidic channels by in situ polymerisation, leading to monolithic materials being increasingly utilised for a larger variety of purposes in micro-fluidic platforms. Applications of porous polymer monoliths, silica-based monoliths and related homogeneous porous polymer gels in the preparation of separation columns, ion-permeable membranes, preconcentrators, extractors, electrospray emitters, micro-valves, electrokinetic pumps, micro-reactors and micro-mixers in micro-fluidic devices are discussed herein. Procedures used in the preparation of monolithic materials in micro-channels, as well as some practical aspects of the micro-fluidic chip fabrication are addressed. Recent analytical/bioanalytical and catalytic applications of the final micro-fluidic devices incorporating monolithic materials are also reviewed.     

阿苯达唑的微波-循环伏安法测定

以玻碳电极为工作电极,在微波作用下采用循环伏安法研究了阿苯达唑的电化学特性,结果表明微波可以增大阿苯达唑的氧化峰电流,据此建立了一种新型检测阿苯达唑的电化学方法。在优化实验条件下,无微波作用时,响应电流与阿苯达唑的浓度在4.0×10-5~1.0×10-3mol/L范围内呈线性关系,线性方程为Ip(μA)=8.303 6c(mmol/L)+0.727 1(r=0.999 3,n=7),检出限为1.78×10-5mol/L;在80 W微波作用下,阿苯达唑的峰电流增大近1倍,响应电流与阿苯达唑的浓度在2.0×10-5~1.0×10-3mol/L范围内呈线性关系,线性方程为Ip(μA)=15.41c(mmol/L)+1.435 9(r=0.998 9,n=8),检出限为1.01×10-5mol/L。研究表明,微波-循环伏安法测定阿苯达唑具有较高的选择性和灵敏度,且样品处理简单快速,用于阿苯达唑片的测定,结果满意。     

葛根素的循环伏安测定及其电化学行为研究

在0.02 mol/L NH4Cl-NH3.H2O(pH8.0)的底液中,采用循环伏安法测定葛根素,得到一良好的氧化峰,峰电位Ep=+0.57V,峰电流Ip与葛根素的浓度在1.046×10-7～5.767×10-5mol/L范围内成线性关系,相关系数r为0.9989,检出限为1.046×10-7mol/L.测定葛根中葛根素的含量,平均回收率在99.8%.并且研究了葛根素在玻碳电极上的电化学行为,结果表明葛根素的电极过程具有吸附性和不可逆性.     

不同钙基CO_2吸收剂的循环特性研究

对石灰石和白云石这两种不同钙基CO2吸收剂的循环特性进行了实验研究,考察了晶格结构不同的钙基CO2吸收剂,随着循环次数的增加,吸收剂的表面形态、分子孔径及比表面积等微观结构的变化,分析了影响吸收剂不同衰减趋势的主要原因。结果表明,白云石基B-CaO吸收剂循环吸收容量稳定性明显高于石灰石基C-CaO吸收剂;白云石中含有的MgO起到原子骨架的作用,减少吸收过程中由于生成碳酸钙产品层引起的孔堵塞,从而有效的保持了吸收剂的活性。     

Synthesis of 12-aryl-1-oxo-1,2,3,4,5,12-hexahydroindolo-[2,1-b]quinazoline-6-carbonitriles by recyclization of 11-aryl-1-oxo-2,3,4,5,10b,11-hexahydro-1H-indolo[2,3-b]quinoline-10b-carbonitriles

A general and convenient method for the synthesis of 12-aryl-1-oxo-1,2,3,4,5,12-hexahydroindolo[2,1-b]quinazoline-6-carbonitriles was proposed. The method is based on the recyclization of 11-aryl-1-oxo-2,3,4,5,10b,11-hexahydro-1H-indolo[2,3-b]quinoline-10b-carbonitriles. The structure of 12-(3-methoxyphenyl)-8-methyl-1-oxo-1,2,3,4,5,12-hexahydroindolo[2,1-b]quinazoline-6-carbonitrile was studied by X-ray diffraction analysis.     

The Inclusion Complex of Ferrocene with a Dithiolene Functionalized β-Cyclodextrin

A new cyclodextrin derivative with the anion side-arm, mono[6-deoxy-6-(2-sodium thio-1,2-dicyane ethylenylthio)]-cyclodextrin (6-mnt-CD), and its inclusion complex with ferrocene (6-mnt-CD/Fc), have been prepared and characterized by elemental analysis, IR spectroscopy, UV spectroscopy, mass spectrometry, ¹³C-NMR spectroscopy, thermogravimetry, and cyclic voltammetry (CV). Thermogravimetry analysis of the compound shows that the thermal stabilities of both the host and the guest in the inclusion complex have been greatly improved due to an additional interaction between the side-arm of the host and the guest. The interplay between the guest and the host with side-arm in the complex resulted in smaller positive potential shifts in CV compared to that in the inclusion complex CD/Fc.     

Electrochemistry of the bis(1,4,7-triazacyclodecane) cobalt(III) complex and its role in the catalytic reduction of hydrogen

The electrochemistry of the bis(1,4,7-triazacyclodecane) cobalt(III) complex at a mercury electrode, HMDE, in aqueous Britton–Robinson buffer solutions was investigated using cyclic voltammetry, double-potential-step chronoamperometry and chronocoulometry. The cyclic voltammetric data were analyzed by digital simulation to confirm and to measure the heterogeneous and homogeneous parameters for the suggested electrode mechanism. Generally, the complex is electrochemically reduced giving rise to two cyclic voltammetric waves. The first wave is a diffusion-controlled reversible wave. It is assigned to the stable Co(III)/Co(II) redox couple. The second one is found to be irreversible and corresponding to a reduction of Co(II) to Co(I) species. The monovalent cobalt, highly unstable, is rapidly protonated, and then forms cobalt hydride. The hydride decomposes to hydrogen molecules and regenerates Co(II) species following a disproportionation pathway. The overall reduction mechanism is concluded to be an EECC kinetics.     

Synthesis, structure and redox potentials of biologically active ferrocenylalkyl azoles

The syntheses, structures, electrochemical properties of the series of ferrocenylalkyl azoles, FcAlkAz, as well as the antitumor activity of ferrocenylmethyl benzimidazole (8) have been studied. Above mentioned compounds were investigated by the method of cyclic voltametry. All of them exhibited a reversible one-electron oxidation-reduction wave owing to the ferrocene-ferrocenium redox couple with a positive shift (0.50-0.65 V) compared with that of ferrocene (0.42 V). The X-ray determination of molecular structures of 1-(ferrocenylmethyl)imidazole (4), 1-(ferrocenylbenzyl)imidazole (7) and 1-(ferrocenylmethyl)bezimidazole (8) was carried out. Compound 4 with imidazolyl substituent was found to be present in N-protonated form. Antitumor activity of 1-(ferrocenylmethyl)benzimidazole (8) against some solid tumor models such as adenocarcinoma 755 (Ca755), melanoma B16 (B16) and Lewis lung carcinoma was studied. The antitumor activity of compound 8 was compared with cisplatin effectiveness against some experimental tumor systems.     

Effect of Surface Structure on Behavior of RuO2 Electrodes in Sulfuric Acid Aqueous Solution

The electrochemical properties of RuO₂ electrodes are studied by means of cyclic voltammetry, potential step, and impedance measurements in aqueous 0.5 mol/dm³ H₂SO₄ as a supporting electrolyte solution and applying the hanging electrolyte meniscus technique. Two types of the electrodes are used: bulk as-grown single-crystal having (101) exposed interface and 500 nm film produced by reactive RF magnetron sputtering at 450°C. The surface structure of the RuO₂ electrodes prepared by different techniques is defined from X-ray LAUE backscattering. Experimental data show that, for both RuO₂ electrodes, the charging components include a slow diffusion-controlled contribution, due to proton injection–ejection. The diffusion characteristics and the diffusion coefficients for the same electrodes are estimated and reported.