Hydrothermal Synthesis and Electrochemical Properties of Complex Cu(CH3C6H4COOH)2(2,2''-bipy)·(H2O)

The title complex has been synthesized by 4-methylbenzoic acid and 2,2'-bipyridine (bipy) in the mixed solvent of water and methanol. It crystallizes in the triclinic system, space group (P1-) with a = 0.7047(3), b = 1.1217(5), c = 1.6718(7) nm, α = 103.826(7), β = 90.772(6), γ = 104.195(6)°, C26H25CuN2O5.50, Mr = 517.02, V = 1.2404(9) nm3, Dc = 1.384 g/cm3, Z = 2, F(000) = 536, μ(MoKα= 0.921 mm-1, R = 0.0782 and wR = 0.2172. Structural analysis shows that the copper atom is coordinated with three oxygen atoms from two 4-methylbenzoic acids and one water molecule together with two nitrogen atoms from 2,2'-bipyridine, giving a distorted square-pyramid coordination geometry. The cyclic voltametric behavior of the complex has also been described.     

CLONING, EXPRESSION AND CHARACTERIZATION OF Pro3 GENE OF YEAST Saccharomyces cerevisiae

The proline biosynthetic pathway and Pro genes in Saccharomyces cerevisiae have just begun to be studied recently. In our laboratory, Pro2 gene of S. cerevisiae had been cloned in yeast. As described in this paper, yeast Pro3 gene was also cloned, which can complement yeast Pro3 mutants, and be expressed efficiently in E. coli. The high activities of this gene product, L-pyrroline-5-carboxylate (P5C) reductase, can be detected in both organisms. The activity of the Pro3 gene product in multiple copy plasmids is not higher than that of single copy genes in chromosomes in both yeast and E. coll. The preliminary characterization of the gene is also reported.     

Synthesis and Crystal Structur of (4,4''-H2bipy)[CdBr4]·H2O

The title compound (4,4'-H2bipy)[CdBr4]·H2O 1 has been synthesized via hydrothermal reaction and characterized by X-ray diffraction. The crystal belongs to monoelinic,space group P21/c with a=8.260(3), b=23.926(7), c=9.774(2) (A), β=106.777(9)°,C10H12Br4CdN2O, Mr=608.26, V=1849.4(9)(A)3, Z=4, Dc=2.185 g/cm3, S=1.005, μ(MoKα)=9.814 mm-1, F(000)=1128, R=0.0646 and wR=0.0989. The crystal structure analysis of 1reveals that the title compound features an isolated structure, based on discrete 4,4'-H2bipy moieties and lattice water molecules which are linked by hydrogen bonds together with tetrahedral cadmium atoms terminally coordinated by four bromine atoms.     

配合物[Cu2(m-MBA)4(2，2′-bipy)2(H2O)]·H2O的水热合成、晶体结构及电化学分析

A copper(Ⅱ) complex [Cu₂(m-MBA)₄(2，2′-bipy)₂(H₂O)]·H₂O with m-methylbenzoic acid (m-MBA), 2,2′-bipyridine (2,2′-bipy) and water molecule has been synthesized by means of hydrothermal way and characterized. Crystal data for this complex: monoclinic, space group C2/c, a=2.591 8(5) nm, b=1.414 2(3) nm, c=1.790 8(4) nm, β=131.80(3)°, V=4.893 3(17) nm³, D_c=1.379 g·cm^-3, Z=4, F(000)=2 104 , Final GooF=1.034, R₁=0.065 6, wR₂=0.197 6. The crystal structure shows that two neighboring copper(Ⅱ) ions are linked together by two bridging-chelating m-methylbenzoic acid groups, one bridging water molecule, forming a cage structure and the Cu(Ⅱ)-Cu(Ⅱ) bond distance is 0.366 7 nm. Each copper(Ⅱ) ion is coordinated with two nitrogen atoms of one 2,2′-bipyridine molecule and four oxygen atoms from three m-methylbenzoic acid molecules and one water molecule, repectiveley, forming a distorted octahedral coordination geometry. The cyclic voltammetric behavior of the Complex was also investigated. CCDC: 648619.     

三环己基锡吡啶酸甲酯的合成、结构、热稳定性及其量子化学计算研究

利用吡啶-3-甲酸与Cy3SnOH反应合成了[(C5H4N)COOSnCy3]n,经元素分析、1H NMR、IR和X-射线衍射表征分子结构。在该配合物的结构中,中心Sn原子呈现五配位畸变三角双锥构型,并通过分子间的N→Sn配位形成一维链状线型聚合物,分子链间的C-H…O氢键作用将配合物分子组装成三维超分子网络结构。利用量子化学G03W软件,在LANL2DZ基组对配合物的稳定性、前沿分子轨道组成及能量进行研究。热重分析表明该化合物在273℃开始发生分解。     

高表面能晶面裸露的金属氧化物微纳米晶体的可控合成

表面结构是影响固体材料物理和化学性质的重要因素,由于高表面能的晶面上存在更多的表面悬挂键等,高表面能晶面裸露的微纳米晶体一般表现出很好的物理和化学活性．近年来,科研工作者针对高能面微纳米晶体材料的制备及性能调控进行了大量的研究工作并取得了一定的进展．本文重点讨论了高能面裸露的金属氧化物半导体微纳米晶体的合成制备方法．主要以本课题组近年在该领域的研究为例,分别从晶体生长过程中的静电作用法、“帽”式试剂保护法、过饱和度调控法、动力学调控法及选择性化学刻蚀法等几个方面对高表面能晶面裸露的金属氧化物微纳米晶体的制备进行了系统的总结．     

扑热息痛在Nafion-石墨烯-纳米金复合膜修饰电极上的电化学行为

利用Nafion,石墨烯(GS)和纳米金(AuNs)的N,N-二甲基甲酰胺(DMF)分散液制备了一种新型纳米复合膜修饰碳糊电极(CPE),建立了一种测定扑热息痛(PCT)的新方法。采用扫描电镜(SCE)对修饰电极进行了表征;利用循环伏安法(CV)研究了PCT在修饰电极上的电化学行为。利用微分脉冲溶出伏安法(DPSV)优化了测定PCT的试验条件。结果表明:PCT在Nafion/GS/AuNs修饰电极上于0.43V处出现了一灵敏的氧化峰(Epa),其电极过程受扩散控制。同时利用氧化峰可以进行微量PCT的检测,其峰电流(ip)与PCT浓度(c)在0.5～10μmol/L和10～900μmol/L范围内均呈良好的线性关系,相关系数分别为0.9968和0.9973,检出限(S/N=3)为0.1μmol/L。复合膜修饰电极稳定性较好,可用于实际药品中扑热息痛的含量的快速检测。     

双酚A在壳聚糖石墨烯复合膜电化学传感器上的电化学行为及测定

采用hummers法制备了石墨烯,以碳糊电极为基底电极采用滴涂法制备了壳聚糖石墨烯复合膜电化学传感器(CTS/GR/CPE),并利用循环伏安法和线性扫描溶出伏安法研究了双酚A在电化学传感器上的电化学行为。在pH 7.4的磷酸盐缓冲液中,于-0.1V富集180s后,该电化学传感器对双酚A具有良好的电催化作用,于0.564V处有一灵敏的氧化峰,线性范围为1.00×10-6～7.00×10-5mol/L和7.00×10-5～1.00×10-3mol/L,检出限(S/N=3)为1.00×10-7mol/L。方法用于塑料制品中溶出双酚A的测定,回收率为96.4%～100.5%。     

二苄基锡水杨醛缩邻氨基苯酚Schiff碱配合物的合成、结构及荧光性质研究

二苄基二氯化锡和水杨醛缩邻氨基苯酚Schiff碱按物质的量比1∶1反应,合成了二苄基锡水杨醛邻缩氨基苯酚Schiff碱配合物。经X-射线衍射方法测定了其晶体结构,属单斜晶系,空间群为P21/n,晶体学参数a=1.110 03(3)nm,b=1.719 87(5)nm,c=1.176 09(3)nm,β=100.564 0(10)°,V=2.207 23(10)nm3,Z=4,Dc=1.541 g·cm-3,μ(Mo Kα)=11.81 cm-1,F(000)=1 023,R1=0.026 8,wR2=0.061 9,中心锡原子为五配位的畸变三角双锥构型。对其结构进行量子化学从头计算,探讨了配合物的稳定性、分子轨道能量以及部分前沿分子轨道的组成特征。研究了配合物的荧光性质。     

基于银纳米粒子/氧化石墨烯复合薄膜制备TNP电化学传感器

利用改进的Hummers法制备了氧化石墨烯(GO), 以葡萄糖为还原剂直接在GO表面沉积银纳米粒子(AgNPs)得到性能稳定的AgNPs/GO纳米复合材料;基于该纳米复合材料修饰电极构建了一种新型的2, 4, 6-三硝基苯酚(TNP)电化学传感器。采用原子力显微镜(AFM)、扫描电镜(SEM)、透射电镜(TEM)、紫外可见光谱(UV-Vis)和交流阻抗(EIS)等多种方法对纳米复合薄膜进行了表征;并研究了TNP在复合薄膜修饰电极上的电化学行为和动力学性质。结果表明, AgNPs/GO对TNP有较强的电催化活性, 在复合薄膜修饰电极出现一灵敏的氧化峰和3个还原峰;利用氧化峰可对TNP进行定量分析。同时整个电极过程明显不可逆, 电极反应受到吸附步骤控制;复合膜电极表面覆盖度为5.617×10^-8 mol·cm^-2, 在所研究电位下的速率常数为9.745×10^-5 cm·s^-1。在pH 6.8的磷酸缓冲液中, 当富集电位为-0.70 V, 富集时间为60 s;TNP氧化峰电流与其浓度在5.0×10^-9~1.0×10^-7 mol·L^-1范围内成良好线性关系, 相关系数为0.995 8, 检出限可达1.0×10^-9 mol·L^-1。所制备的电化学传感器稳定性和选择性较好;用于实际水样中TNP的现场快速检测, 加标回收率在 97.6%~103.9%之间。