Stereochemical effects in mass spectrometry. Part 10-reaction mass spectrometry of cyclic glycols and monosaccharides with methylene chloride as reagent gas

The reaction mass spectrometry of cyclic glycols and monosaccharides with methylene chloride as reagent was studied. In the presence of ammonia, it was found that methylene chloride reacted stereoselectively with the quasi-molecular ions of cyclic glycols and monosaccharides to form characteristic ions, by comparison of the relative abundances of which the stereoisomers of cyclopentane-l,2-diols and cyclohexane-l,2-diols and some monosaccharides could be definitely distinguished.     

catena‐Poly­[[tetra­aqua­iron(II)]‐μ‐succinato‐κ2O:O′]

The title complex, {[Fe(C₄H₄O₄)(H₂O)₄]}_n, is an infinite poly­meric compound bridged by the succinate dianion. Two carboxyl­ate groups coordinate in a monodentate manner to the Fe^II atom, in a trans fashion, with an O—Fe—O bond angle of 175.72 (6)° and Fe—O distances of 2.0886 (14) and 2.1008 (15) Å. One of the uncoordinated carboxyl­ate O atom forms an intramolecular hydrogen bond with a coordinated water mol­ecule. Extensive hydrogen bonding between parallel poly­meric complex chains results in a three‐dimensional supramolecular structure.     

Particle Interactions in Diffusiophoresis and Electrophoresis of Colloidal Spheres with Thin but Polarized Double Layers

The diffusiophoretic and electrophoretic motions of two colloidal spheres in the solution of a symmetrically charged electrolyte are analyzed using a method of reflections. The particles are oriented arbitrarily with respect to the electrolyte gradient or the electric field, and they are allowed to differ in radius and in zeta potential. The thickness of the electric double layers surrounding the particles is assumed to be small relative to the radius of each particle and to the gap width between the particles, but the effect of polarization of the mobile ions in the diffuse layer is taken into account. A slip velocity of fluid and normal fluxes of solute ions at the outer edge of the thin double layer are used as the boundary conditions for the fluid phase outside the double layers. The method of reflections is based on an analysis of the electrochemical potential and fluid velocity disturbances produced by a single dielectric sphere placed in an arbitrarily varying electrolyte gradient or electric field. The solution for two-sphere interactions is obtained in expansion form correct to O(r(12)(-7)), where r(12) is the distance between the particle centers. Our analytical results are found to be in good agreement with the available numerical solutions obtained using a boundary collocation method. On the basis of a model of statistical mechanics, the results of two-sphere interactions are used to analytically determine the first-order effect of the volume fraction of particles of each type on the mean diffusiophoretic and eletrophoretic velocities in a bounded suspension. For a suspension of identical spheres, the mean diffusiophoretic velocity can be decreased or increased as the volume fraction of the particles is increased, while the mean electrophoretic velocity is reduced with the increase in the particle concentration. Generally speaking, the particle interaction effects can be quite significant in typical situations. Copyright 2000 Academic Press.     

Ion Recognition and Analytical Application of a Fibroin Modified Electrode

A novel fibroin modified electrode with ion recognition was reported. The membrane with isoelectric point of pH 4.5, was modified on graphite and carbon fiber electrodes. The pH-responsive ion recognition of the modified electrode was investigated by use of some neurocompounds. The fibroin carbon fiber electrode has been used for in-vivo determination.     

Understanding effect of wall structure on the hydrothermal stability of mesostructured silica SBA-15

Mesostructured silica SBA-15 materials with different structural parameters, such as pore size, pore volume, and wall thickness, etc., were prepared by varying the postsynthesis hydrothermal treatment temperature and adding inorganic salts. The hydrothermal stabilities of these materials in steam (100% water vapor) were systematically investigated using a variety of techniques including powder X-ray diffraction, transmission electron microscopy, nitrogen sorption, and (29)Si solid-state NMR. The effect of the pore size, microporosity or mesoporosity, and wall thickness on the stability was discussed. The results show that all of the SBA-15 materials have a good hydrothermal stability under steam of 600 degrees C for at least 24 h. N(2) sorption measurements show that the Brumauer-Emmett-Teller surface area of SBA-15 materials is decreased by about 62% after treatment under steam at 600 degrees C for 24 h. The materials with thicker walls and more micropores show relatively better hydrothermal stability in steam of 600 degrees C. Interestingly, we found that the microporosity of the mesostructured silica SBA-15 is a very important factor for the hydrothermal stability. To the materials with more micropores, the recombination of Si-O-Si bonds during the high-temperature steam treatment may not cause direct destruction to the wall structure. As a result, SBA-15 materials with more micropores show better stability in pure steam of 600 degrees C. Nevertheless, these materials are easily destroyed in steam of 800 degrees C for 6 h. Two methods to effectively improve the hydrothermal stability are introduced here: one is a high-temperature treatment, and another is a carbon-propping thermal treatment. Thermal treatment at 900 degrees C can enhance the polymerization degree of Si-O-Si bonds and effectively improve the hydrothermal stability of these SBA-15 materials in 800 degrees C steam for 12 h. But, this approach will cause very serious shrinkage of the mesopores, resulting in smaller pore diameter and low surface area. A carbon-propping thermal treating method was employed to enhance the polymerization of Si-O-Si bonds and minimize the serious shrinkage of mesopores at the same time. It was demonstrated to be an effective method that can greatly improve the hydrothermal stability of SBA-15 materials in 800 degrees C steam for 12 h. Furthermore, the SBA-15 materials obtained by using the carbon-propping method possess larger pores and higher surface area after the steam treatment at 800 degrees C compared to the materials from the direct thermal treatment method after the steam treatment.     

CAHN－2000磁天平的调试与数据处理系统的研制

叙述了ＣＡＨＮ－２０００磁天平（美国）调试过程中如何解决液氮温区的测试，自制了磁天平与计算机的接口，编写了数据采集、处理和控制等高原 软件，节省了几万美元，部分指标超过原配套水平，三年来仪器在对国同外开放过程中，液氮温区的工作一直正常，实测了上千个样品，提供的数据已撰写数十篇文章在国内外刊物上发表。由此说明，要充分发挥进口仪器的使用效率，必须对仪器的工作原理、结构特点有透乇的了解，同时要有相当的自     

Counterpoise技术和He-H2O配合物的平衡几何

在得到MP4, SCF的关于总能量及结合能的四个势能面的基础上,着重分析了电子相关作用, 消除基函数超位误差的Counterpoise(CP)技术对van der Waals配合物He-H2O的平衡几何的影响并得到了更精确的平衡几何预测。     

金属载体催化剂的涂层研究

在高温氧化处理不同时间的金属载体箔片上涂覆MgAl2O4/Al2O3过渡涂层,利用TG-DSC,XRD,SEM,BET和超声振动等分析测试技术,对载体和涂层的微观结构与表面特性进行研究.结果表明,在950 ℃下高温氧化5 h,箔片表面生成板状Al2O3晶须,有利于增强涂层与箔片的附着力.在载体表面涂覆一层MgAl2O4/Al2O3过渡涂层,有助于提高活性组分与金属载体的结合力,可以获得高结合强度的涂层结构,促使活性元素高度分散.     

Novel calix[4]arene-thiacrown ether for selective and efficient extraction of Ba(II), Pb(II), and Hg(II)

A di-ionizable p-tert-butylcalix[4]arene-1,3-thiacrown-5 ether extractant was synthesized. Its cone conformation and polyether ring attachment regioselectivity were verified by NMR spectroscopy. The metal ion-complexing properties of this ligand were evaluated by solvent extractions of metal cations from aqueous solutions into chloroform. The ligand was found to be an efficient extractant with Ba²⁺ selectivity in competitive solvent extraction of alkaline earth metal cations. It also exhibits high extraction ability for Pb²⁺ and for Hg²⁺ in single species solvent extractions.