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在凝胶体系NaX(F、Cl、Br)Na2OAl2O3SiO2CTAB(十六烷基三甲基溴化铵)H2O中,研究了水热合成中孔MCM41的合成条件。实验证明,在398K下晶化8~16d,NaX/SiO2介于0.01~0.05时,均可合成出MCM41分子筛;NaF的加入,可以加快MCM41分子筛的晶化速度;NaBr的加入,对形成MCM41分子筛有阻碍作用。采用XRD、SEM、TGDTA和N2吸附对合成样品加以表征,证明合成样品具有介孔分子筛特性。 相似文献
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Jinxiang Li Ayaka Ogasawara Tamao Odake Tomonari Umemura Kin-ichi Tsunoda 《Analytical sciences》2004,20(12):1673-1679
A new isoelectric focusing (IEF) system for two-dimensional polyacrylamide gel electrophoresis (2-D PAGE) has been proposed. In this system, a super-soft and tough IEF gel was achieved by casting polyacrylamide gel down to 2.0% T using a loose multifilament string (LMS) of nylon as a gel support. The IEF apparatus for the LMS-gel, fabricated from acrylic boards, had a cooling water chamber, and eliminated the need of electrode solutions by directly connecting the two ends of individual gels to platinum electrodes. The carrier ampholyte-generated pH gradients using the new IEF system was stable over a long duration of time and a wide range of voltages, and the IEF time became shorter using a 2.0% T gel than using a 4.0% T gel. Also, the LMS-gels prepared in different runs exhibited excellent reproducibility. The new IEF system was applied to 2-D PAGE of a chicken skeletal muscle extract, and it was found that the protein loading capacity, protein entry into the LMS-gels, and protein transfer efficiency from the first-dimensional to the second-dimensional gels were significantly improved by using a low-concentration (2.5% T) gel. Also, proteins of high molecular weight of more than 200 kDa were observed in the 2-D maps, and therefore the new IEF system has a very good potential to be applied for fast 2-D PAGE of high molecular-weight proteins. 相似文献
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A concise and efficient protocol for the first synthesis of ferrocene‐containing allenes based on the homologation reaction of ferrocenylacetylene and aldehydes promoted by ZnI2 was developed. The present method was applicable to many kinds of substituted aldehydes, providing good to excellent yields of ferrocene‐containing allenes. Copyright © 2012 John Wiley & Sons, Ltd. 相似文献
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Yanping Gao Xiaohua Gao Jinxiang Zeng Jian Yin 《International journal of environmental analytical chemistry》2013,93(7):521-533
A novel method for the determination of Pb2+ with bismuth film electrodes (BFEs) based on magneto-voltammetry was investigated. In the presence of a 0.6?T external magnetic field, square wave voltammetry of Pb2+ was performed with BFEs. A high concentration of Fe3+ was added to the analytes to generate a large cathodic current during the preconcentration step. A Lorentz force from the flux of net current through the magnetic field resulted in convection. Then, more Pb2+ deposited onto the electrode and larger stripping peak currents were observed. BFEs that were prepared by simultaneously depositing the bismuth and Pb2+ on an electrode offered a mercury-free environment for this determination. This method exhibits a high sensitivity of 4.61?µA?µM?1 for Pb2+ over the 1?×?10?8 to 1?×?10?6?M range. A detection limit as low as 8.5?×?10?10?M was obtained with only 1-min preconcentration. The method was successfully applied to determine Pb2+ in real water samples. 相似文献
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Silica‐particle‐supported zwitterionic polymer monolith for microcolumn liquid chromatography
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A silica‐particle‐supported zwitterionic polymeric monolithic column, shortened as supported column (S‐column), was prepared by the in situ polymerization of methacrylic acid, ethylene dimethacrylate, and 2‐(dimethylamino)ethyl methacrylate in the presence of a ternary porogenic solvent containing water, methanol, and cyclohexanol in a 250 μm id fused‐silica capillary prepacked with 5 μm bare silica particles. In the S‐column, a thin layer of the polymers was formed around the silica particles in the form of nanoglobules, leaving the interstitial spaces between the particles free for liquid flow. The effects of the preparation conditions on the morphology of the monolith were investigated by scanning electron microscopy and backpressure measurements. The selected volumetric ratio of porogens, monomer concentration, polymerization time, and temperature are 1:1:8 (water/methanol/cyclohexanol), 25% v/v, 5 h, and 60°C, respectively. The S‐column was evaluated by comparison with its conventional organic counterpart in terms of morphology, mechanical stability, permeability, swelling–shrinking behavior, capacity, and efficiency. The results demonstrate that the S‐column is superior to its counterpart in all the terms with the exception of permeability. The above merits and zwitterionic property of the S‐column were further confirmed by separate separations of four inorganic anions and three organic cations. 相似文献
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通过液相法合成了Cu2O纳米立方体, 并在其基础上利用金属有机框架化合物(MOFs)的自组装形貌调控, 进一步构建了层级多孔Co3O4和氮杂碳双壳层的Cu2O/Co3O4@C异质结构复合材料. 利用X射线衍射(XRD)、 扫描电子显微镜(SEM)、 透射电子显微镜(TEM)、 热重分析(TGA)、 BET比表面积及孔径分析、 拉曼光谱和X射线光电子能谱(XPS)等表征手段证实了Cu2O/Co3O4@C异质结构复合材料的成功构筑. 双壳层结构设计和丰富的层级孔道结构有效抑制了材料在充放电循环过程中的体积膨胀, 材料在循环100次后仍保持了原有的形貌和构造. 表面多孔结构对电解液的充分浸润、 异质结构的界面内建电场以及缺陷氮杂碳的表面包覆有效提升了材料的电子和离子导电能力. 异质结构设计、 形貌调控、 多孔特性和氮杂碳的协同作用, 使得Cu2O/Co3O4@C复合材料呈现出优异的电化学性能, 在0.1 A/g电流密度下的首次放电比容量达到2065 mA·h/g, 在 2 A/g电流密度下的可逆放电比容量高于360 mA·h/g, 在1 A/g电流密度下循环350次后仍有530 mA·h/g的高可逆放电比容量. 相似文献