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    24 December 1990, Volume 6 Issue 4
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    Articles
    Synthesis and Magnetic Properties of Copper (Ⅱ) Complexes with Pyridine N-Oxide-2-ylmethy-lidenedithiocarbazate as Ligands
    Gou Shaohua, You Xiaozeng, Xu Zheng, Zhu Duolin, Yu Yunpen
    1990, 6(4):  255-261. 
    Abstract ( )   PDF (460KB) ( )  
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    Aseries of copper (Ⅱ) complexes with pyridine N- oxide- 2- ylmethylidened-ithiocarbazates as ligands were synthesized and characterized by IRspectra, electronic spectra and magnetic moments measurement at room temperature. Variable temperature magnetic susceptibilites (3-300K) of four complexs were measured and fitted with the Bleaney-Bowers dimer equation by considering the magnetic interaction between molecules. The fitting results show the existence of intramolecular ferromagnetic interactions and intermolecu-lar anti-ferromagnetic interactions in these copper( Ⅱ) complexes.
    Crystal and Molecular Structure of Copper (Ⅱ) Dimeric Complex of S-Methyl-β-N-(Pyridine N-Oxide-2-ylmethylidene) Dithiocarbazate with Acetonitrile
    Yu Kaibei, Zhou Zhongyuan, Gou Shaohua, You Xiaozeng, Xu Zheng
    1990, 6(4):  262-265. 
    Abstract ( )   PDF (266KB) ( )  
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    The crystal and molecular structure of copper(Ⅱ) dimeric complex of S-methyl-B-N-(pyridine N-oxide-2-ylmethylidene) dithiocarbazate with acetonitrile, [CuL(CH3CN)]2(ClO4)2, was determined by X-ray diffraction. The complex crystalizes in monoclinic system with space group P21/n, a= 7.685(2), 6=20.160(6), c= 10.847(5) Å,B=107.89(3), Z=2,Dc=1.788g/cm3, F(000)=835.8, u= 18.17 cm-1(Moka,R= 0.057.Each Cu(Ⅱ) ion in the complex is surrounded by a distorted square pyramidal. The basal plane is comprised of S, Nand Oatoms of one ligand together with a Natom of the solvent--acetonitrile, while the axial position is occupied by the Satom of the other ligand. The bond length of Cu-S(bridging) is 3.038A. and Cu-Cu distance is 3.700A.
    Synthesis and Properties of u-Oxamido Heterobinuclear Cu(Ⅱ)-Co(Ⅱ) Complexes
    Liao Daizheng, Zhang Zhiyong, Jiang Zonghui, Hao Sonqi, Wang Genglin
    1990, 6(4):  266-270. 
    Abstract ( )   PDF (363KB) ( )  
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    Three heterobinuclear complexes were synthesized, namely [Cu(oxpn) Co(L)2] (ClO4)2·xH2O(L= 2,2'-bipyridyl(bpy), 1,10-phenanthroline(phen) , and 5-nitro-1, 10-phenanthroline (NO2-phen)), where oxpn represents N, N'-bis(3-aminopropyl) oxam-ido. Based on 1R, elemental analysis, conductivity measurement and electronic spectra, these complexes were characterized by an extended oxamido-bridged structure with Cu(Ⅱ) in a planar environment and Co(Ⅱ) in a octahedral environment. The symmetry of the cation is very close to C2v.The complexes were also characterized with variable temperature (4～300K) magnetic susceptibility, and the data were fit for the susceptibility equation derived from spin Hamilton, H= -2JS1·S2-DSx12 by least square strategy. The exchange integral, J, was found to be -22.36cm-1 (for bpy);-15.45cm-1 (for phen); -19.10cm-1(for NO2-phen), indicating that there is a weak antiferromagnetic spin-exchange interaction between the metal ions.
    Synthesis and Crystal Structure of Tri(8-quinolinol) Yttrium-Tri(8-quinolinol) Nickel Perchlorate [YQ(HQ)2][NiQ3](ClO4)
    Zhang Mingjie, Huang Chunhui, Xu Guangxian
    1990, 6(4):  271-275. 
    Abstract ( )   PDF (358KB) ( )  
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    The title compound was synthesised and the X-ray diffraction analysis shows that the crystal belongs to in monoclinic system, space group P21/n with α=16.972(4) A ,b=14.128(3)A , c=22.615(4)A ,β=103.16(2)°,V=528.14A3,F(000)=2264, Z=4. Both cation [YQ(HQ)2]2+ and anion [NiQ3]- are of distorded octahedral geometry with coordination number of 6. Its IRspectrum was recorded.
    A Study of Retention Time Gradient Effect of Gradientally Loaded Columns
    Yun Xiqin, Kou Dengmin, Li Yanhong, Lu Xianyu
    1990, 6(4):  276-280. 
    Abstract ( )   PDF (299KB) ( )  
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    In this work, the "retention time gradient effect" of gradient GCcolumns is intensively studied to establish some equations and formulas for structure calculation of chromatographic columns. In addition, the relevant computer programs are designed.
    Chemometrics:Research on Basic Algorithms and Their Applications
    Yu Ruqin
    1990, 6(4):  281-288. 
    Abstract ( )   PDF (607KB) ( )  
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    Some aspects of the fundamental problems of chemometrics are reviewed based on the research work undertaken in this laboratory. The topics touched upon Include analytical information theory, experimental design and optimization, sampling, analytical detection theory, calibration, signal processing, chemical pattern recognition, quantitative structure-activity relationships, digital simulation, and teaching chemometrics as a chemical discipline.
    A New Expert System for Structural Interpretation of IR Spectra
    Cheng Lingran, Zhang Maosen
    1990, 6(4):  289-294. 
    Abstract ( )   PDF (403KB) ( )  
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    Anew expert system has been developed which can be used to aid chemists in structural interpretation of infrared spectra. The system consists of five essential portions: knowledge-base , inference engine, database, knowledge-acquisition module and explanatory interface. The system is implemented in Turbo PROLOGartificial intelligence language. Compared with other spectral interpretation systems this system is of the following advantages, i. e. the system has a friendly user interface, two kinds of methods for managing toowledge-base, several useful explanatory facilities such as why and how should explanation be made, etc. ; in addition, it can be run on the IBM PC/XTand its compatible microcomputers. Another important feature of the system is that it can simulate the reasoning procedure by which experienced chemists may interpret spectra as well as deduce complete molecular structures. So the system can also be used as a helpful learning tool for training chemistry students in IRspectrum interpretation and organic structure elucidation.
    Biosensors Based on the Tissue of Plant as Catalytic Material for Amino Acids
    Qi Deyao, Zhuang Yunlong, Chi Qijin
    1990, 6(4):  295-299. 
    Abstract ( )   PDF (349KB) ( )  
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    Two tissue electrodes are described in this paper. It is shown that a portion of intact tissue from apple or cactus can be coupled with potentiometric ammonia gas sensing electrode to prepare sensors for some amino acids with good response properties. Their optimum operating conditions and properties with respect to buffer sort, pHof the bulk solution, selectivity, linearity, stability, sensitivity and response time are studied and discussed. At the same time, the dynamic parameters, such as Km and Vm, of L-glutamine deaminasc and L-as-paragine deamlnase have been obtained by means of these tissue electrodes.
    Studies on Lattice Parameter,Molar Volume and Excess Molar Volume of Pb-based a-phase Solid Solution in Pb-Sn-Cd Ternary System
    Liu Hengli, Long Xiang, Kang Hongye, Zhao Muyu
    1990, 6(4):  300-306. 
    Abstract ( )   PDF (479KB) ( )  
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    The lattice parameters a and the molar volumes Vm of Pb-based a-phase solid solutions in the Pb-Sn-Cd ternary system were determined by means of X-ray diffraction. The lattice parameters a vary linearly with the molar fractions, the molar volumes show a positive deviation from the ideal solution behaviour, and the contribution of the solute Cd to the excess molar volumes Vm is much larger than that of the solute Sn. According to Vegard' s law orsub-regular solution model, the relationship between the experimental data of a or Vm andthe compositions of alloy is obtained by the mathematic regressive method, the prediction precisions of the both formulae are within the limits of experiment error.
    Extraction and Structure Investigation of the Poly-saccharides from the Pollen of Typha Angustifolia L.
    Miao Ping, Lin Yao, Jin Sheng
    1990, 6(4):  307-312. 
    Abstract ( )   PDF (440KB) ( )  
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    Three polysaccharides, TAA, TAB, TAChave been isolated from the pollen of Typha angustifolia L., and purified by hot water extraction, alcohol precipitation, Sevage method, gel filtration (Sephadex G50) and ion-exchange chromatography on DEAE Sephadex A25 and DEAE-cellulose. Their purities were tested by gel filtration and electrophoresis. Their structures were characterized by paper chromatography of the hydrolysis products, GLCanalysis of the alditol acetates, alkylation analysis, 1H NMRand 13C NMRspectra. TAAis mainly composed of a-L-arabinofuanose, β-D-galactose and α-D-galacturonic acid, while the backbones of TABand TACare composed of (1→5)-linked α- L-arabinofuranosyl residues.
    An ESR Study on Singlet Oxygen Photoproduction of the Meso-Tetrakis-(Substituted Phenyl) Porphine Derivatives
    Chen Jiyao, Lu Yameng, Chen Shiming, Cai Hualxin, Xu Deyu, Wang Shaoyin
    1990, 6(4):  313-316. 
    Abstract ( )   PDF (2335KB) ( )  
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    The ability of meso-tetrakis-(substituted phenyl) porphine derivatives for photo-generating singlet oxygen (O2) is studied by ESRspectrometry. The results show that the singlet oxygen yields of most of porphine derivatives are higher than that of HPD. It is also exhibited that the nature and structure of the substituent at the meso position are closely related to the photo-sensitizing ability of meso-tetrakis-(substituted phenyl) porphine.
    Sol-Gel Distribution of Polycondensation Reaction
    Li Zesheng, Ba Xlnwu, Sun Jiazhong, Tang Xinyi
    1990, 6(4):  317-319. 
    Abstract ( )   PDF (221KB) ( )  
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    Atheoretical approach to polycondensation reaction of Aa-Bb type Involving intramolecular cycllzatlon has been proposed by Tang Au-chin et al.. In this paper, the theoretical sol-gel distribution is tested by polycondensation of adipic acid with trimethylol propane in a sto-ichiometric ratio of 0.8, and the effect of intramolecular cyclization is discussed in detail.
    WO3 Anodic Oxide Film——I. Electrochromism and Auto-bleaching mechanism
    Lin Zhonghua, Chen Kunyao, Zheng Zhizhen, Chen Haiyi
    1990, 6(4):  320-326. 
    Abstract ( )   PDF (502KB) ( )  
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    Electrochromic and auto-bleaching processes at the WO3 anodic film in 0.5 mol/L H2SO4 solution were investigated by cyclic voltammetry, a. c. impedance technique and photocurrent spectrometry. The colouration mechanism consists of hydrogen adsorption on the WO3 surface and the transport of Hatoms in the WO3 lattice. The bleaching process involves at least two steps: transport of interstitial Hatoms and hydrogen desorption on the Wsurface, resulting in interstitial H+ ions; then extration of the H+ ions driven by the external electric field. The auto-bleaching arises from the hydroxylation due to both partial interstitial Hatoms and a little of water contained in the film.
    Studies on Cyclodextrin Inclusion Complex by Fluorescence Anisotropy
    Jiang Yunbao, Huang Xianzhi, Chen Guozhen
    1990, 6(4):  327-331. 
    Abstract ( )   PDF (369KB) ( )  
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    An equation for determining the equilibrium association constant (KA) of cyclodextrin inclusion complex with fluorescence anisotropy is derived and used to determine KAof pyrene-B-cyclodextrin inclusion complex. The existing forms of cyclodextrin inclusion complex in solution, the interaction type of host with guest, and the possibility of application of B-cyclodextrin in the analysis of metal ions using naphthalene derivative as a ligand are discussed based on the equation derived along with the curve of fluorescence anisotropy versus cyclodextrin concentration of guest/cyclodextrin system.
    Isomorphous Substitution of Metallic Elements for Zeolite Y in the Aqueous Solution
    Tang Yi, Xu Jinsuo, Gao Zi
    1990, 6(4):  332-340. 
    Abstract ( )   PDF (678KB) ( )  
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    The substitutions of Ti, Fe and Zr into zeolite Yin the aqueous solutions of (NH4)2TiF6, (NH4)3ZrF7 and (NH4)3FeF6 were systematically Investigated. It was found that Ai atoms in the framework can be replaced by some metallic elements and the extent of substitution depends on the M/A1 ratio of the solution. The maximum allowable M/A1 ratio of the aqueous solution Is related with the radius of the Matom and the stability constant of the MFnm- complex. The substituted zeolite samples with crystallinity greater than 80% were characterized by means of XRD, IR, DTA, TPRand NH3-TPDmeasurements. The incorporation of Ti, Fe and Zr into the zeolite leads to an increase in the unit cell parameter, a lowering of thermal stability and a red shift of the asymmetric stretching frequency. The extent of these changes is apparently related with the ionic radius of the metallic element and the degree of substitution. The results of various characterization methods show that the het-eroatoms are readily Introduced into the zeolite framework by this preparation method. It was also observed that the substitution of heteroatoms may strengthen or weaken the surface acidity of zeolite Y.
    The Photovoltage-gas Sensitive Properties of 7,7,8,8-Tetracyanoquinodimethane(TCNQ)
    Jiang Lei, Wang Dejun, Liu Wang, Chai Xiangdong, Li Tiejin
    1990, 6(4):  341-345. 
    Abstract ( )   PDF (362KB) ( )  
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    In this paper, surface photovoltage technique (SPV) was applied to the study of photovoltaic and gas sensitive properties of TCNQpolycrystal. It was found that SPVshows two peaks at 390 nm(P1) and 480 nm (P2) in the ultraviolet-visible range. And they are opposite in phase. The results of gaseous adsorption confirm that P2 shows the acceptor characteristics, while P1 shows that of donor. During adsorption, donor gas interacts with conjugated II* orbital, acceptor gas with the terminal group C=N .
    XPS,Chemical Trapping, and DRFTIR Study on Mechanism of By-Products Formation in Selective (AMM)Oxidation of Propylene on MoO3 and γ-Bi2MoO6
    Weng Weizheng, Yan Jiyang, Cai Junxiu, Dai Shenjun,Cao Shoujing, Chen Lingling, Wan Huilin
    1990, 6(4):  346-353. 
    Abstract ( )   PDF (592KB) ( )  
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    XPSand chemical trapping experments with H2, NH3, and CH3Ias trapping agents were carried out for studying the adsorption of propylene over MoO3 or γ-Bi2MoO6. The results show that the fragmentation of carbon chain takes place during the adsorption of propylene through breaking C -Cdouble bond and C-Cbond on Mo2+ and the adjacent lattice oxygen, leading to formation of the oxygen- or nitrogen-containing by-products of C1 and C2 species. Diffuse-Reflection Fourier Transform Infrared (DRFTIR) Spectroscopy was used to study the surface species formed during the chemisorption and reaction of propylene over y-Bi2MoO6 at a lower temperature. The results that C1, C2 adspecies were detected by DRFTIRat 175℃ are consistent with the results of XPSand chemical trapping experiments, whlle the results at 50℃ Grasselli et al.
    A Kinetic Study on Dismutation of Superoxide Ion by Macrocyclic Dioxotetramine-Copper(Ⅱ) Complex by Using Pulse Radiolysis
    Shen Mengchang, Luo Qinhui, Zhu Shourong, Tu Qingyun, Dai An bang, Liu Andong, Ou Hongchun, Li Fengmei, Di Shaojie
    1990, 6(4):  354-359. 
    Abstract ( )   PDF (461KB) ( )  
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    We studied the reaction kinetics of dismutation for superoxide ion by copper (Ⅱ) complex of macrocycllc dioxotetramine ligand 12- ( 4'-nitro )- benzyl-1,4,7,10-tetraazacy-clotridecane-11,13-dionato copper (Ⅱ) by using pulse radiolysis. The rate constants of dismutation kcat's were measured to be 1.78×106mol-1·L·s-1(at pH 7.8) and 1.06×106mol-1·L·s-1(at pH 7.8). The reaction mechanism is similar to that catalyzed by super-oxide dismutase.
    A Stochastic Extension of Macroscopic Stability Criterion of Nonequilibrium Steady State in Chemical Reaction Systems Governed by Master Equation
    Luo Jiuli
    1990, 6(4):  360-369. 
    Abstract ( )   PDF (683KB) ( )  
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    By means of both the separation of the perturbation in accordance with characteristic parnmeters and the Kramers Moyal-expansion of the master equation, it is shown that the time derivative of the partial excess quantity of stochastic entropy due to the deviation from the most probable path is related to the responsibility of a system to the external macroscopic perturbations. This evolution rate of the partial excess stochastic entropy is equivalent to the partlal excess stochastic entropy production, as well as the stochastic excess entropy production rate based on the stochastic potential npproach. It appears also as an eqivalent quantity of the Gibbs excess entropy production for the Polsson distribution. The macroscopic stability of chemical reaction systems is dominnted by this new stochastic quantity when the local equilibrium thermodynamics is broken down .
    Polymer Radii and Moments in the Polycondensation Reaction of Aa Type
    Li Zesheng, Sun Jiazhong, Ba Xinwu, Tang Aoqing
    1990, 6(4):  370-372. 
    Abstract ( )   PDF (248KB) ( )  
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    For the polycondensation reaction of A. type, the kth radius for k>2 can be expressed in terms of polymer moments.
    Separation of Neutral Amino Acids with Ligand Exchange Resins
    Wang Shouting, Wang Busen, He Binglin
    1990, 6(4):  373-377. 
    Abstract ( )   PDF (348KB) ( )  
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    Four neutral amino acids (Gly, Ala,.Val and Leu) were separated with ligand exchange resins. The separation capacity of the ligand exchange resins is compared with that of common ion exchange resins. The effects of eluent, column temperature, and central metal ions of the support on the separation are studied. The relationship between matrix structure of resins and their separation capacity is analysed.
    Specific Interactions in a Variety of Multicomponent Polymers
    Jiang Ming
    1990, 6(4):  378-385. 
    Abstract ( )   PDF (747KB) ( )  
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    For a variety of multicomponent polymers including simple blends, block copolymers, IPNs, lonomer blends, homopolymer/block copolymer blends and composites composed of Inorganic particles and polymer matrix, the current situation and trend of introducing specific Interactions and its effect on the misclbility and properties of the systems have been reviewed with emphasis on the recent results obtained in the author' s laboratory.
    Studies on Pervaporation Separation of Ethanol/Water Mixtures with Membranes of Polypropylene Sulfonate Salts
    Lin Shaokun, Xu Yingbin, Lin Shangan
    1990, 6(4):  386-390. 
    Abstract ( )   PDF (490KB) ( )  
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    Sulfonated polypropylene membranes loaded with different kinds of counter-ions were prepared by heterogeneous chiorosulfonation reaction of polypropylene membrane followed by hydrolysis and ion-exchange reaction. The membranes obtained were used for selective separation of ethanol/water mixtures by pervaporation. The effects of counter-ion species, ion-exchange capacity, solution composition, thickness of membrane and temperature on the separation behavior of the membranes were investigated. Microstructure and morphology of the membranes were examined by X-ray and SEMas well.
    Quantitative Study on the Templating Effect in the Formation of ZSM-5 Molecular Sieve
    Song Tianyou, Xu Ruren
    1990, 6(4):  391-393. 
    Abstract ( )   PDF (209KB) ( )  
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    Luminescence Centers in BaFCl:Ce3+ and BaFCl:Gd3+ Crystals
    Su Mianzeng, Liao Chunshen
    1990, 6(4):  394-398. 
    Abstract ( )   PDF (341KB) ( )  
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    A Facile Synthesis of 5-Monosubstituted Isopropylidene Malonates
    Huang Xian, Wu Jlnlong
    1990, 6(4):  399-401. 
    Abstract ( )   PDF (216KB) ( )  
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    Preparation of Cationic Starch by Electromagnetic Dry Process (EMDP)
    Yue Shitai, Zhang Lijun
    1990, 6(4):  402-404. 
    Abstract ( )   PDF (308KB) ( )  
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