稀土高氯酸溶液导数光谱的研究及其在分析中的应用 Ⅶ.四阶导数分光光度法直接测定混合稀土氧化物中镱和镝

本文在近红外光区研究了镱(Ⅲ)和镝(Ⅲ)1mol/L HClO_4溶液的四阶导数吸收光谱,认真选择了仪器操作条件,提高了测定镱和镝的选择性。通过校正系数法,使镱的光度法测定成为可能,克服了在可见光区测定镝需要校正干扰的缺点,达到在混合稀土中直接测定镱和镝的目的。     

In-channel indirect amperometric detection of nonelectroactive anions for electrophoresis on a poly(dimethylsiloxane) microchip

In the present paper, we describe a microfluidics-based sensing system for nonelectroactive anions under negative separation electric field by mounting a single carbon fiber disk working electrode (WE) in the end part of a poly(dimethylsiloxane) microchannel. In contrast to work in a positive separation electric field described in our previous paper (Anal. Chem. 2004, 76, 6902-6907), here the electrochemical reduction reaction at the WE is not coupled with the separation high-voltage (HV) system, whereas the electrochemical oxidation reaction at the WE is coupled with the separation HV system. The electroactive indicator is the carbon fiber WE itself but not dissolved oxygen. This provides a convenient and sensitive means for the determination of nonelectroactive anions by amperometry. The influences of separation voltage, detection potential, and the distance between the WE and the separation channel outlet on the response of the detector have been investigated. The present detection mode is successfully used to electrochemically detect F-, Cl-, SO4(2-), CH3COO-, H2PO4-. Based on the preliminary results, a detection limit of 2 microM and a dynamic range up to three orders of magnitude for Cl- could be achieved.     

取代邻苯二腈的合成

在室温条件下合成了一系列芳氧基邻苯二腈化合物,应用无素分析、1HNMR、IR确定了它们的结构,讨论了不同取代基对反应的影响.结果表明,酚的芳环上有推电子基时反应容易进行;酚的芳环上有拉电子基时反应慢或不反应.     

Probing the local structure and mechanical response of nanostructures using force modulation and nanofabrication

Nanostructures of self-assembled monolayers (SAMs) are designed and produced using coadsorption and nanografting techniques. Because the structures of these artificially engineered domains are predesigned and well-characterized, a systematic investigation is possible to study the mechanical responses to force modulation under atomic force microscope tips. Force modulation imaging reveals characteristic contrast sensitivity to changes in molecular-level packing, molecule chain lengths, domain boundaries, and surface chemical functionalities in SAMs. By means of actively tuning the driving frequency, the resonances at the tip-surface contact are selectively activated. Therefore, specific surface features, such as the edges of the domains and nanostructures or desired chemical functionalities, can be selectively enhanced in the amplitude images. These observations provide a new and active approach in materials characterization and the study of nanotribology using atomic force microscopy.     

无水醋酸镍与水杨醛肟固相配位反应的热化学研究

用新型的具有恒定温度环境的反应热量计，以６ｍｏｌ·ｄｍ－３ＨＣｌ溶液为量热溶剂，分别测定了ＨＳＡＯ，Ｎｉ（Ａｃ）２和Ｎｉ（ＳＡＯ）２，ＨＡｃ先后溶于该溶剂的溶解焓．设计了一个新的热化学循环，计算得到该配位反应的反应焓ΔｒＨ＝－８６．０７５ｋＪ·ｍｏｌ－１，并估算出了ΔｆＨ［Ｎｉ（ＳＡＯ）２，２９８Ｋ］＝－４０１．３３６ｋＪ·ｍｏｌ－１．     

THE SEPARATION,PURIFICATION AND DECOLORIZATION OF NEW ANTIBIOTICS-MILUPEINAN USING ADSORPTION RESIN

1. INTRODUCTION Fig.1 The Chemical Structure of Milupeinan As a new type of antibiotics Milupeinan, not only possesses antibacterial activities against a wide range of Gram-positive and Gram-negative bacteria, but also higgh stability under th…     

制备高比表面积碳化硅的几种影响因素

采用溶胶凝胶法，以蔗糖和正硅酸乙酯(TEOS)为原料，草酸为TEOS水解的催化剂，制备均相碳化硅前驱体，在氩气氛和高温条件下(1 350～1 600 ℃)将碳化硅先驱体进行碳热还原，制备出高比表面积的SiC。考察了水/TEOS物质的量的比、碳/硅物质的量的比及镍盐等因素对碳化硅比表面积的影响。结果表明，当n_water/n_TEOS=7.5，n_C/n_Si=4时，适宜的镍催化剂(n_Ni/n_TEOS=0.005)，凝胶形成的时间最短，镍盐的加入可使碳热还原温度降低200 ℃。     

A new C21-steroidal glycoside from Cynanchum stauntonii

A new C21-steroidal glycoside with two known compounds were isolated from the root of Cynanchum Stauntonii.Based on thespectral analysis,including MS,1H NMR,13C NMR,DEPT,1H-1H COSY,13C-1H COSY,HMQC and HMBC,their chemicalstructures were determinated as glaucogenin-C 3-O-a-L-cymaropyranosyl-(1→4)-b-D-digitoxopyranosyl-(1→4)-β-D-canaropyranoside(1),stigmasterol(2)and ursolic acid(3).     

气相色谱质谱联用仪与微机的数据传输和处理

报道了一种用于气相色谱质谱联用仪和微机之间实现数据传输和处理的方法。方法可更有效地利用质谱仪采集的数据，解决了工作站处理数据的局限性。经数据格式转换，原始数据可以在微机上实现色谱峰再现，从而为色谱条件的优化和定量数据处理创造了条件。     

Photocatalytic Oxidation of Aniline in the Gas Phase Using Porous TiO2 Thin Films

The gas-phase photocatalytic oxidation of aniline on a new kind of porous nano-TiO₂ composite films is investigated. The composite film was prepared on glass fiber with the water glass as binders and dilute H₂SO₄ solution as solidifying reagent. The surface characters were observed by scanning electron microscope. The photocatalytic degradation of aniline on the composite films was carried out in a TiO₂/UV system. Some important factors affecting the photodegradation, such as the concentration of TiO₂, the initial concentration of aniline, and the existing water vapor, are also studied. The product of photocatalytic oxidation was detected by Fourier transform-Infrared. The partial intermediate products were absorbed on TiO₂ surface, which resulted in catalyst deactivation. But when it was irradiated under UV illumination or solar irradiation for some time, the catalyst could be reused without loss of catalytic activity. Translated from the Journal of Wuhan University (Natural Science Edition), 2005, 51(2) (in Chinese)