Access to the structures of fluoromagnesium compounds: synthesis and structural characterization of the β-diketiminato magnesium fluoride [{CH(CMeNAr)2}Mg(μ-F)(THF)]2·toluene

β-Diketiminato magnesium fluoride [{CH(CMeNAr)₂}Mg(μ-F)(THF)]₂·toluene (Ar=2,6-i-Pr₂C₆H₃, 2·toluene) was synthesized. The molecular structure of 2 revealed for the first time, the double fluoro bridge feature between the two magnesium atoms with a typical MgF bond length (average 1.95 Å).     

Catalytic Adsorptive Stripping Voltammetry of Germanium(IV) in the Presence of Gallic Acid and Vanadium(IV)‐EDTA

A highly sensitive and selective catalytic adsorptive cathodic striping procedure for the determination of trace germanium is presented. The method is based on adsorptive accumulation of the Ge(IV)‐gallic acid (GA) complex onto a hanging mercury drop electrode, followed by reduction of the adsorbed species. The reduction current is enhanced catalytically by addition of vanadium(IV)‐EDTA. The optimal experimental conditions include the use of 0.03 mol/L HClO₄ (pH1.6), 6.0×10^?3 mol/L GA, 3.0×10^?3 mol/L V(IV), 4.0×10^?3 mol/L EDTA, an accumulation potential of ?0.10 V(vs. Ag/AgCl), an accumulation time of 120 s and a differential pulse potential scan mode. The peak current is proportional to the concentration of Ge(IV) over the range of 3.0×10^?11 to 1.0×10^?8 mol/L and the detection limit is 2×10^?11 mol/L for a 120 s adsorption time. The relative standard deviation at 5.0×10^?10 mol/L level is 3.1%. No serious interferences were found. The method was applied to the determination of germanium in ore, mineral water and vegetable samples with satisfactory results.     

Inhibition of the toxic byproduct during photocatalytic NO oxidation via La doping in ZnO

It is of a great challenge to develop semiconductor photocatalysts with potential possibilities to simultaneously enhance photocatalytic efficiency and inhibit generation of toxic intermediates.In this study,we developed a facile method to induce the La doping and cationic vacancie(V(Zn))on ZnO for the highly efficient complete NO oxidation.The photocatalytic NO removal efficiency increases from 36.2%to 53,6%.Most importantly,a significant suppressed NO2 production also has been realized.According to the DFT calculations,ESR spectra and in situ FTIR spectra,the introduction of La^3+induce the redistribution of charge carriers in La-ZnO,which promote the production of·O2^- and lead to the formation of V(Zn)for the formation of·OH,contributing to the complete oxidation of NO to nitrate.Besides,the conversion pathway of photocatalytic NO oxidation has been elaborated,This work paves a new way to simultaneously realize the photocatalytic pollutants removal and the inhibition of toxic intermediates generation for efficient and safe air purification.     

3,5-diBr-DMPAP直接光度法测定葡萄糖酸锌含量

为建立一种快速、简便、灵敏测定葡萄糖酸锌含量的方法,在非离子型表面活性剂聚氧乙烯异辛基苯基醚(TritonX-100)存在下,用2-(3,5-二溴-2-吡啶偶氮)-5-二甲氨基酚(3,5-diBr-DM-PAP)作显色剂,直接光度法测定了葡萄糖酸锌。结果表明,该法显色络合物最大吸收波长为560 nm,线性范围为0~1.5μg.mL-1,表观摩尔吸光系数为1.10×105L.mol-1.cm-1,回收率为98.7%~102.2%,具有操作快速、简便,结果灵敏可靠等优点,应用该法直接测定补锌口服液葡萄糖酸锌含量,结果满意。     

Coaxial electrospinning core-shell fibers for self-healing scratch on coatings

Polystyrene (PS) fibers with core-shell structure were prepared by coaxial electrostatic spinning using liquid epoxy or curing agent as the core and PS solution as the shell. Scratch self-healing coatings were realized by using the healant-loaded core-shell fibers in the matrix.     

树枝状十二酯的合成

以乙二胺和丙烯酸十二酯为原料，甲醇为溶剂，采用迈克尔加成反应合成了低代的树枝状十二酯。探讨了反应条件对树枝状十二酯收率的影响。乙二胺2mL(30mmol)，n(乙二胺)：n(丙烯酸十二酯)=1：6，甲醇占反应液总体积的50％，反应温度40℃，反应时间48h，产率54．9％。     

Two New C—21 Steroidal Glycosides from Cynanchum aurichulatum

Two new C-21 steroidal glycosides, cynanauriculoside I and cynanauriculoside Ⅱ, were isolated from the roots of Cynanchum aurichulatum. Their structures were established using spectroscopic methods including one and two-dimensional NMR.     

CdS/SiO2复合材料的低频Raman散射研究

对用溶胶凝胶法制备的ＣｄＳ／ＳｉＯ２复合材料进行低频Ｒａｍａｎ散射研究，结果表明可从其低频Ｒａｍａｎ散射峰位计算出ＣｄＳ微晶的粒径，两种不同的低频振动模式由激发光的两种偏振方向加以区分，低频Ｒａｍａｎ散射射的二级散射峰根据实验结果加以指认，所得平均粒径结果与透射电镜观察结果有较好的对应关系，复合材料吸收光谱吸收边蓝移与ＣｄＳ纳米子粒径之间存在着密切的关系，实验证明，样品吸收边能量与ＣｄＳ平均粒径的     

Baker''''s yeast mediated reduction of substituted acenaphthenequinones: Regio-and enantioselective preparation of mono-hydroxyacenaphthenones

Baker's yeast mediated reduction of acenaphthenequinone within 4-10 h afforded mono-hydroxyacenaphthenone mainly with low enantioselectivity, the substrate and mono-hydroxyacenaphthenone product almost converted to dihydroxyacenaphthene after 48 h. By control of the reaction time and in the presence of DMF as co-solvent, the reduction of 6-substituted acenaphthenequinones under vigorous agitation afforded the corresponding 2-hydroxyacenaphthenones in 24-84% yields with 10-93% ee.     

聚乙二醇在高真空条件下的单链弹性

在过去二十年间，高分子的单链弹性已经得到了广泛的研究.然而由于环境和高分子之间往往有着复杂的相互作用，实验中很难得到高分子在严格无扰状态下的单链弹性（即本征弹性）.为此，利用单分子力谱技术研究了高真空条件下聚乙二醇（PEG）的单链弹性.结果表明，由于高真空条件下溶剂分子的干扰被消除，PEG在这一准无扰状态下呈现其本征弹性.在非极性有机溶剂中，由于溶剂分子和PEG之间只有微弱的范德华力作用，PEG表现出和高真空中基本一致的弹性.然而，在不同环境中，力曲线的低力区（F<100 pN）存在着细微的差异.这一现象可归因于不同条件下基底与PEG链之间的吸附力不同.采用的高真空力谱可用于研究其他高分子单链在准无扰状态下的本征弹性.