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Silylated and acetylated β-cyclodextrins for gas chromatographic stationary phases

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Journal of Central South university of Technology 2001年第4期8卷 239-243页

作者： TANG Ke wen 1,2.,YI Jian ming 2.ZHOU Chun shan 1,ZHONG Shi an 1 (1. college of chemistry and {2. Engineering, Central South university, changsha 410083, China 2. college of chemistry and {2. Engineering, Yueyang Normal university college of chemistry and {2. Engineering Central South University Changsha China college of chemistry and {2. Engineering Yueyang Normal University Yueyang China

Two new chiral stationary phases, 2.3 di O acetyl 6 O trimethylsilyl β cyclodextrin (DATBCD) and 2.6 di O trimethylsilyl 3 O acetyl β cyclodextrin(DTABCD), were synthesized, their structures were identified by means of infrared and NMR spectra. Capillary columns were coated with the two stationary phases by dynamic method. The chromatographic properties, and enantiomers separation, such as ketone, esters, alcohols and olefines, were investigated on the silylated and acetylated β cyclodextrin stationary phases. The experimental results show that the silylated and acetylated β cyclodextrins are suitable to be used as capillary gas chromatographic stationary phases, the relative polarity of DATBCD and DTABCD stationary phases is respectively 4143 and 392., the column efficiencies are respectively 3084 and 4198, and DATBCD is of stronger enantioselectivity than DTABCD, capacity factor of the first eluted enantiomer ( k 1) and separation factor(α)of α phenylethanol on DATBCD stationary phase are respectively 8.2. and 1.019.

关键词： capillary gas chromatography silylated and acetylated β-cyclodextrins enantiomeric separation

Effect of static magnetic field on activity of immobilized α-amylase

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Chinese Science Bulletin 1997年第2期42卷 127-130页

作者： YAN Liushui, ZHU Yuanbao, HE-Shuang’e and CAO Zhixiang1 Department of chemical Engineering, Nanchang Institute of Aeronautical Technology, Nanchang 330034, China 2. Department of chemistry and chemical Engineering, hunan university, changsha 410082. China Department of chemical Engineering Nanchang Institute of Aenwututical Techndogy Nanchang China Department of chemistry and chemical Engineering Hunan University Changsha China

BIOLOGICAL effect of magnetic field is one of the three major subjects of contemporary biomagnetism, and is also the basis of applied biomagnetism. In order to explore magnetic biological effects, the influence of various sorts of magnetic field on many living systems as well as their different constructural levels has been extensively studied. However, only a few studies with in vitro enzyme have been reported, and few researches concerning the influence of magnetic field on immobilized enzyme reactions have been published. This note describes

关键词： static magnetic field immobilized α-amylase enzyme activity oscillatory behaviour.

Resolution of α-cyclohexyl-mandelic acid enantiomers by two-phase (O/W) recognition chiral extraction

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Science China chemistry 2007年第6期50卷 764-769页

作者： TANG KeWen1,2. ZHANG GuoLi2. HUANG KeLong2. LI Yuanjian3 & YI JianMin1,2.1 Department of chemistry and chemical Engineering, {2. Institute of Science and Technology, Yueyang 414000, China 2.college of chemistry and chemical Engineering, Central South university, changsha 410083, China 3 college of Pharmaceutical Science, Central South university, changsha 410078, China Department of chemistry and chemical Engineering Hunan Institute of Science and Technology Yueyang China college of chemistry and {2. Engineering Central South University Changsha China college of Pharmaceutical Science Central South University Changsha China

This paper presents a new chiral separation technology:two-phase(O/W)recognition chiral *** behavior of alpha-cyclohexyl-mandelic acid enantiomers was studied in the extraction system with D(L)-isobutyl tartrate in 1,2.dichloroethane organic phase and beta-CD derivatives in aqueous phase,and the influence of the kind and concentration of extractant and pH on extraction performance was *** experimental results indicate that two-phase(O/W)recognition chiral extraction is of strong chiral separation ***-^-CD,HE-beta-CD and Me-beta-CD have higher recognition ability for S-CHMA than that for R-CHMA,among which HP-beta-CD has the strongest ability;whereas,D-isobutyl tartrate has reversed recognition ability for *** the extraction system containing HP-beta-CD and D-isobutyl tartrate,e.e.% of S-CHMA in aqueous phase reached 2..6% by one stage extraction,and the distribution ratio for R-CHMA(k_R)and for S-CHMA(k_S)and separation factor(alpha)are 2.44,0.89 and 2.49,***,pH and concentration of extractant have great effects on chiral separation ***-phase(O/W)recognition chiral extraction has great significance for preparative separation of racemic compounds.

关键词： two-phase(W/0)recognition chiral extraction alpha-cyclohexyl-mandelic acid enantiomers

Aspects of recent developments in analytical chemometrics

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Science China chemistry 2006年第3期49卷 193-203页

作者： LIANG Yizeng1,2. WU Hailong1, SHEN Guoli1, JIANG Jianhui1, LIANG Sheng2.& YU Ruqin1 1. State Key Laboratory of Chemo/Biosensing and Chemometrics, college of chemistry and {2. Engineering, hunan university, changsha 410082. China 2. Research Center of Modernization of Traditional Chinese Medicines, Central South university, changsha 410081, China State Key Laboratory of Chemo/Biosensing and Chemometrics College of Chemistry and Chemical Engineering Hunan University Changsha China Research Center of Modernization of Traditional Chinese Medicines Central South University Changsha China

Some aspects of recent developments in analytical chemometrics are discussed, in par- ticular the developments viewed from the angle of the research efforts undertaken in authors’ labora- tories. The topics concerned include resolution of high-order chemical data, morphological theory and methodology for chemical signal processing, multivariate calibration and chemical pattern recognition for solving complex chemical problems, and resolution of two-way chemical data from hyphenated chromatographic instruments.

关键词： chemometrics, high-order chemical data, pattern recognition, multivariate calibration and resolution.

Preparation of well-defined polystyrene/silica hybrid nanoparticles by ATRP

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Science China chemistry 2008年第1期51卷 51-57页

作者： OU BaoLi1,2.LI DuXin2.1 college of chemistry and {2. Engineering,hunan university of Science and Technology,Xiangtan 4112.1, China 2.State Key Laboratory of Powder Metallurgy,Central South university,changsha 410083, China college of chemistry and {2. Engineering Hunan University of Science and Technology Xiangtan China State Key Laboratory of Powder Metallurgy Central South University Changsha China

Immobilization of the atom transfer radical polymerization (ATRP) macroinitiators at the silica nanoparticle surfaces was achieved through surface modification with excess toluene-2.4-diisocynate (TDI), after which the residual isocyanate groups were converted into ATRP macroinitiators. Structurally well-defined polystyrene chains were grown from the nanoparticle surfaces to yield individual particles composed of a silica core and a well-defined, densely grafted outer polystyrene by ATRP, which was initiated by the as-synthesized silica-based macroinitiator. FTIR, NMR and gel permeation chro-matography (GPC) were used to characterize the polystyrene/silica hybrid particles.

关键词： silica nanoparticles surface modification atom transfer radical polymerization polystyrene hybrid particle

Adsorption and corrosion inhibition behavior of imidazole on cobalt electrodes studied by SERS and electrochemical methods

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Science China chemistry 2005年第6期48卷 497-503页

作者： GU Wei1, LIU Guokun2. REN Bin2. WU Deyin2. GU Renao1 & TIAN Zhongqun2.1. Department of chemistry, college of chemistry and chemical Engineering, Suzhou university, Suzhou 2.5006, China 2. State Key Laboratory for Physical chemistry of Solid Surfaces and Department of chemistry, college of chemistry and chemical Engineering, Xiamen university, Xiamen 361005, China Department of chemistry College of Chemistry and Chemical Engineering Suzhou University Suzhou China State Key Laboratory for Physical chemistry of Solid Surfaces and Department of chemistry College of Chemistry and Chemical Engineering Xiamen University Xiamen China

The interaction of imidazole with Co electrodes in an electrochemical system was studied by surface-enhanced Raman scattering (SERS) and electrochemical methods. The SER spectra of Co in an imidazole solution as a function of the applied potential were analyzed and the assignment of the Raman bands was made. It was found that there were three kinds of sur-face species on the Co surface in different potential regions and they were interchangeable de-pending on the potential. In a relatively negative potential region (?1.2.to ?0.9 V), imidazole was adsorbed on the surface and its orientation might change from a vertical configuration via the N-end of the pyridine ring to a tilted configuration via the C2.N3 double bond. In a more positive potential region (?0.8 to ?0.7 V), the SERS signal from the adsorbed imidazole weakened and finally disappeared, meanwhile the signal from the Co and imidazole complex strengthened gradually. At the open circuit potential (?0.6 V), we detected very strong bands from the Co ox-ides. By comparing the Tafel curves of the Co electrode in the solution without and with imidazole, we found that imidazole has a marked effect on the corrosion inhibition of the Co electrode. This result demonstrates that we may be able to reveal the complicated interaction of surface species with metal surface at the molecular level by combining the SERS and electrochemical methods.

关键词： cobalt, imidazole, inhibition, surface-enhanced Raman spectroscopy, Tafel plot.

Preparation of polystyrene/silica nanocomposites by radical copolymerization of styrene with silica macromonomer

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Science China chemistry 2007年第3期50卷 385-391页

作者： OU BaoLi1,2.& LI DuXin2.1 college of chemistry and {2. Engineering, hunan university of Science and Technology, Xiangtan 4112.1, China 2.State Key Laboratory of Powder Metallurgy, Central South university, changsha 410083, China college of chemistry and {2. Engineering Hunan University of Science and Technology Xiangtan China State Key Laboratory of Powder Metallurgy Central South University Changsha China

A two-stage process has been developed to generate the silica-based macromonomer through surface-modification of silica with polymerizable vinyl groups. The silica surfaces were treated with excess 2.4-toluene diisocynate (TDI), after which the residual isocyanate groups were converted into polymerizable vinyl groups by reaction with hydroxypropylacrylate (HPA). Thus, polystyrene/silica nanocomposites were prepared by conventional radical copolymerization of styrene with silica macromonomer. The main effecting factors, such as ratios of styrene to the macromonomer, together with polymerization time on the copolymerization were studied in detail. FTIR, DSC and TGA were utilized to characterize the nanocomposites. Experimental results revealed that the silica nanoparticles act as cross-linking points in the polystytene/silica nanocomposites, and the glass transition temperatures of the nanocomposites are higher than that of the corresponding pure polystyrene. The glass transition temperatures of nanocomposites increased with the increasing of silica contents, which were further ascertained by DSC.

关键词： silica nanoparticles surface modification styrene radical copolymerization nanocomposites

A thin-layer spectroelectrochemical study of 3,3',5,5'-tetramethylbenzidine at SnO_2.F film optically transparent electrode

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Science China chemistry 2004年第4期47卷 267-275页

作者： JIAO Kui1, YANG Tao2.& NIU Shuyan1,2.1. college of chemistry and Molecular Engineering, Qingdao {2. of Science and Technology, Qingdao 2.6042. China 2. college of chemistry and chemical Engineering, Ocean {2. of China, Qingdao 2.6003, China Correspondence should be addressed to Jiao Kui college of chemistry and Molecular Engineering Qingdao University of Science and Technology Qingdao China college of chemistry and {2. Engineering Ocean University of China Qingdao China

The electrooxidation of 3,3′,5,5′-tetramethylbenzidine (TMB) is dependent on the pH value of Britton-Robinson (B-R) buffer solution. In this work, the electrooxidation behavior of TMB was investigated with a SnO2.F film optically transparent thin-layer spectroelectrochemical cell. TMB underwent one two-electron electrooxidation process in the pH range from 2.0 to chemical reaction to yield an azo compound. Several spectroelectrochemical techniques, such as thin-layer cyclic voltammetry, thin-layer cyclic voltabsorptometry, thin-layer potential-controlled electrolysis absorptometry, thin-layer single-potential-step chronoabsorptometry, thin-layer dou-ble-potential-step chronoabsorptometry, thin-layer single-potential-step open-circuit relaxation chronoabsorptometry, were applied to this investigation. The formal potential E0’ and the electron transfer number corresponding to the electrooxidation of TMB in B-R buffer solution, and the reaction rate constant of the subsequent chemical reaction were determined.

关键词： 3,3′,5,5′-tetramethylbenzidine tin oxide film optically transparent electrode thin-layer spectroelectro-chemistry electrooxidation

Formation and evolution mechanisms of large-clusters during rapid solidification process of liquid metal Al

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Science China(Physics,Mechanics & Astronomy) 2005年第1期48卷 101-112页

作者： LIU Rangsu, DONG Kejun, LIU Fengxiang, ZHENG Caixing, LIU Hairong & LI Jiyong Department of Applied Physics, hunan university, changsha 410082. China {2. of Materials Science and Engineering, hunan university, changsha 410082. China {2. of chemistry and chemical Engineering, hunan university, changsha 410082. China Department of Applied Physics Hunan University Changsha 410082 China college of Materials Science and Engineering Hunan University Changsha 410082 China college of chemistry and {2. Engineering Hunan University Changsha 410082 China

A molecular dynamics simulation study has been performed for the formation and evolution characteristics of nano-clusters in a large-scale system consisting of 400000 atoms of liquid metal Al. The center-atom method combined with pair-bond analysis technique and cluster-type index method (CTIM) has been applied here to describe the structural configurations of various basic clusters. It is demonstrated that both the 1551 bond-type and the icosahedral cluster (12.0 12.0) constructed by 1551 bond-types are dominant among all the bond-types and cluster-types, respectively, in the system and play a critical role in the microstructure transitions of liquid metal Al. The nano-clusters (containing up to 150 atoms) are formed by the combination of some middle and small clusters with distinctly different sizes, through mutual competition by unceasing annex and evolution in a seesaw manner (in turn of obtaining and losing),which do not occur as the multi-shell structures accumulated with an atom as the center and the surrounding atoms are arranged according to a certain rule. This is the essential distinction of nano-cluster in liquid metal from those obtained by gaseous deposition, ionic spray methods, and so on. Though the nano-clusters differ from each other in shape and size, all of them possess protruding corners that could become the starting points of various dendrite structures in the solidification processes of liquid metals.

关键词： liquid metal, solidification process, large-cluster configuration, evolution mechanism, computer simulation.