The measurements of correlation times of molecules adsorbed on silica gel,alumina and charcoal using NOESY and MAS NMR

The correlation times (τ_c) and cross relaxation rates of toluene, dimethylformamide, tetrahydrofuran, water-acetone and water-dioxane adsorbed on silica gel, alumina and charcoal were obtained by measurements of the integrated intensities of cross and diagonal peaks in their NOESY spectra. The (τ_c) of the above mentioned systems is in the range of 10^?6?10^?9 s, much longer than that in the liquid (10^?12?10^?14 s). It was found that intramolecular rotation of toluene adsorbed on charcoal is slower than that on SiO₂, Al₂O₃ and the inversion of α and β protons in tetrahydrofuran is very fast (τ_c = 1.76×10^?9 s). The cross relaxation plays an important role in the relaxation of molecules adsorbed on solid surfaces with low electron densities.     

纳米二氧化锆制备过程的DSC、TGA和XRD研究

用ＤＳＣ、ＴＧＡ和ＸＲＤ技术研究了在沉淀法制备纳米ＺｒＯ２的过程中，残留ＮＨ４Ｃｌ、ｐＨ值、滴加方式、以及结构稳定剂Ｙ２Ｏ３的添加量对结晶过程的影响。结果表明，残留ＮＨ４Ｃｌ使结晶化温度降低，使放热过程变为吸热过程。而ｐＨ值、滴加方式和结构稳定剂的添加对结晶过程无明显影响。     

活性炭酸处理对CuO／C催化剂上NO还原反应的影响

４种国产活性炭被用于ＮＯ还原反应，其中，山楂核炭和山桃核炭具有较高的ＮＯ还原转化率。实验发现，表面含氧基团－ＣＯＯ－对活性炭自身的还原性和对ＮＯ的还原活性有很重要的影响。对表面富－ＣＯＯ－基团的活性炭，稀盐酸处理使表面－ＣＯＯ－显著分解。     

血卟啉衍生物的色谱分离

本文拟定的纸色谱法是以苯-乙酸乙酯-甲醇-乙酸(9:2:1:1)作展开剂,将血卟啉衍生物(HPD)分离为五部份,分别测定各部份浸取液的荧光发射光谱,作为一种对血卟啉衍生物组份作对比鉴定的参考方法。采用Ward的高效液相色谱程序对比研究结果表明,国产与美国产HPD的组份近似,均以血卟啉为主要组份,而前者血卟啉的含量较高;二者还均含有羟乙基乙烯基衍生物和羟基乙酸酯,初步研究了血卟啉衍生物在甲醇-水溶剂系统中的高效液相色谱行为,进一步将血卟啉衍生物分离为九部份,有利于单一组份研究。     

螺桨烷

本文综述了螺桨烷的最新进展,详细叙述了螺桨烷的合成、结构与性质,特別是小螺桨烷的张力能及桥头-桥头碳-碳单键的价键状态。     

Crystal Structure and Characterization of a Large Polyoxotungstate (NH4)21{La(H2O)5[Ni(H2O)]2As4W40O140}·53H2O

The heteropolytungstate (NH4)₂₁{La(H₂O)₅[Ni(H₂O)]₂As₄W₄₀O₁₄₀}·53H₂O is obtained by the reaction of Na₂₇[NaAs₄W₄₀O₁₄₀]· 60H₂O with NiCl₂·6H₂O, La(NO₃)₃·6H₂O and NH₄Cl at pH‐4.5. The structure and chemical composition are determined by X‐ray diffraction analysis and elemental analysis. The crystal data and main structure refinement are a = 1.9551(3) nm, b = 2.4156(4) nm, c= 3.7068(6) nm, β = 91.505(3)°, V = 17.500 (5) nm³, monoclinic crystal system with space group P2₁/n, Z = 4, R₁ = 0.0573, wR₂ = 0.0717 [I >2<s?(I)], R₁, = 0.2463 and wR₂ = 0.1199 (all data). [La(H₂O)₅] {Ni(H₂O)}₂AS₄W₄₀O₁₄₀ has C₂, symmetry. IR spectra of the ligand [NaAs₄W₄₀O₁₄₀]^27‐ and its three complexes were discussed.     

A Novel Green Preparation of a, a''''-Bis (substituted benzylidene)-cycloalkanones Promoted by FeCl_3 6H-2O in Ionic Liquid

a, a'-Bis(substituted benzylidene)cycloalkanones were efficiently prepared from cycloalkanones and benzaldehydes in [bmim][BF4] by using iron(III) chloride hexahydrate as a catalyst. It is shown that [bmim][BF4] and iron(III) chloride hexahydrate can be quantitatively recovered and be reused effectively for many times. Compared with the known methods, this novel process has the advantage of being an envkonmentally benign process together with good yields and mild reaction conditions.