半导体凝固点测定仪的研制及其应用

为了配合物理化学实验“凝固点降级法测定萘的摩尔质量”,研制出半导体制冷凝固点测定仪,实现了凝固点测定和摩尔质量计算的自动化,解决了老式实验装置存在的问题。通过对环己烷凝固点和萘摩尔质量的测定,验证了该仪器的可靠性,同时还探讨了搅拌速率和冷阱的温度变化对凝固点测定值的影响。     

混合价双核锰[Mn2(cyclen)2(μ-O)2](ClO4)3·4H2O的晶体结构和表征

The mixed-valence manganese(Ⅲ/Ⅳ) complex [Mn2(cyclen)2(μ-O)2](ClO4)3-4H2O (1) (cyclen=1,4,7,10-tetraazacyclododecan) with chemical formula C16H48Cl3Mn2N8O18 has been synthesized and characterized by single crystal X-ray diffraction analysis, elemental analysis, IR and electronic spectra. The results showed that the manganese(Ⅲ/Ⅳ) ions were six-coordinated by four nitrogen atoms from cyclen and two oxygen atoms from the oxygen bridge, forming a distorted octahedron geometry. There were two very strong peaks in the range of 400-700 nm in electronic spectrum, which was similar to Mn catalase and Mn ribonucleotide reductase extracted from organisms.Electrochemical study indicated that the complex underwent a quasi-reversible one-electron reduction and oxidation at E1/2=0.827 V in acetonitrile.     

Crystal Structures and Theoretical Calculation of Zn（Ⅱ） and Cu（Ⅱ） Supramolecular Complexes Based on Macrocyclic Triamine Ligand 1,4,7-Triazacyclodecane （tacd）

Two supramolecular complexes [Zn（tacd）2]（C6H8O4）·6H2O（1） and [Cu（tacd）2]Cl2·4H2O（2） were synthesized and characterized by elemental analysis, IR spectra, TGA and single-crystal X-ray diffraction analysis. The crystal structure showed that the metal ions in complexes 1 and 2 had similar coordination circumstance. But for the complex 2, it formed a novel two-dimensional supramolecular network with 12-membered rings and four-membered rings via hydrogen bond interaction. The thermal gravimetric analyses indicated that the two complexes had similar steps of weight-loss. On the basis of experiment, the two complexes were calculated by DFT-B3LYP/6-31G（d） in Gaussian 03. The results of calculation are in good agreement with the experiment.     

5,10,15,20-四(2-噻吩基)金属卟啉修饰TiO2光催化剂的制备及光催化性能

合成了5,10,15,20-四(2-噻吩基)卟啉(H₂TTP)及它的钴铜锌三种金属卟啉, 并用上述三种金属卟啉分别敏化锐钛矿型的二氧化钛, 制备了CoTTP-TiO₂, ZnTTP-TiO₂, CuTTP-TiO₂三种光催化剂, 对这三种光催化剂进行了扫描电镜(SEM)、X射线光电子能谱(XPS)、紫外-可见漫反射光谱(UV-vis)、红外光谱(IR)的表征. 在300 W汞灯和400 W金卤灯照射下, 制备的光催化剂对4-硝基苯酚溶液的降解表现出比未修饰二氧化钛高的催化效率, 光催化降解反应符合反应一级动力学方程.     

CuSO4(ZnSO4)-CO(NH2)2-H2O三元体系在30℃时的等温溶度研究

报道了CuSO₄(ZnSO₄)-CO(NH₂)₂-H₂O两个三元体系在30℃时的等温溶度及饱和溶液的折光率,绘制了相应的溶度图和折光率-组成图.两个三元体系中分别形成了组成为CuSO₄·3CO(NH₂)₂·H₂O(异成分溶解)和ZnSO₄·CO(NH₂)·2H₂O(同成分溶解)的化合物,并通过元素分析、红外光谱、X射线粉末衍射及热分析对新相进行了表征.     

三元体系MgCl2-CO(NH2)2-H2O在25℃时的等温溶度与新相研究

测定了25℃时三元体系MgCl₂-CO(NH₂)₂-H₂O的等温溶度及饱和溶液的折光率和密度,且绘制成溶度图和性质-组成图.在三元体系内形成2个三元化合物新相:MgCl₂·CO(NH₂)₂·4H₂O(记作A)和Mgcl₂·4CO(NH₂)₂·2H₂O(记作B),B为新化合物.三元体系的溶度图由4支单饱和线[对应单饱和固相为MgCl₂·6H₂O、三元化合物A和B、CO(NH₂)₂]组成,这4支单饱和线两两交于3个三元无变点[对应双饱和固相为MgCl₂·6H₂O+A、A+B、B+CO(NH₂)₂].     

四元体系LiCl-KCl-MgCl2-H2O 25℃时等温研究

本文首次报道了四元体系LiCl-KCl-MgCl₂-H₂O 25℃时的溶度和饱和溶液的折光率、密度和粘度值。并给出了体系的相图、溶度面、总氯量面及上述物理性质面。