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    24 July 1989, Volume 10 Issue 7
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    Articles
    Synthesis and Acidity of B-β Zeolite
    Xiang Shouhe, Wang Qiuying, Wang Jingzhong, Wang Kebing, Li Hexuan
    1989, 10(7):  677-682. 
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    The synthesis of B-β zeolite was studied in the system Na2O-B2O3-SiO2-TEAOH-H2O.The apparent activation energies for nucleation, En, and the activation energy for crystallization, Ec, were calculated on the basis of the crystallization curves.They are 152 kJ·mol-1(ED) and 40 kJ·mol-1 (Ec) respectively.It has been proved that Bis incorporated the framework of Bzeolite during crystallization according to the results obtained from the X-ray diffraction, IRand NMRcharacterization.The acidity of HB-β.was studied by using IRand TPD.B-β has weak acid strength and subsequently has negligible catalytic activity for the n-hexane cracking reaction.However, it exhibits catalytic activity for the cumene cracking reaction.
    Study on Porphyrin Compounds (Ⅸ)——Synthesis of 5-(o-Propenoylaminophenyl)-10,15,20-Triphenyl Porphyrin Polymer and Its Cobalt Complex
    Li Pingying, Jiang Zhaoci, Huang Suqiu
    1989, 10(7):  683-686. 
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    5- (o-propenoylaminophenyl)- 10, 15, 20-triphenylporphyrin (Ⅱ) was synthesized from acryloyl chloride and 5-(o-aminophenyl)-10,15, 20-triphenylporphyrin (Ⅰ) and was further polymerized to 5-(o-propenoylaminophenyl)-10,15,20-triphenylporphyrin polymer(Ⅲ) in the presence of initiator, and the cobalt complexes of (Ⅱ) and (Ⅲ) were also synthesized.Their chemical structures were identified by NMR, UVand IRspectra as well as elemental analysis.
    Formation Mechanism and High Tc Superconductivity of YBa2Cu3O7-δ Thin Film by CSD Method
    Peng Dingkun, Wang Xiandong, Meng Guangyao, Fu Peizhen, Wang Jun, Zhang Yuheng
    1989, 10(7):  687-690. 
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    High Tc superconduction YBa2Cu3O7-δ thin film with zero resistivity temperature higher than85 Kand transition width of 2 Kand thickness of 5 μm,on a substrate of crystal cubic ZrO2, was obtained by using Chemical Spray Deposition (CSD) process.XRD, XPSand SEMetc.were employed to investigate the crystallographic structure, electron structure and micro-morphology of films made under different conditions.The formation mechanism of YBa2Cu3O7-δ, thin film and relation with superconductivity are discussed.
    Selection of Optimal Ratio of Mixed Stationary Phase Column with Computer
    Yang Guangde, Xu Wenguo, Peng Ye, Dong Wen
    1989, 10(7):  691-695. 
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    In this paper, a BASICprogram was designed to calculate the optimal ratio of mixed stationary phase column in GCfor any mixture.Meantime the experimental data of 26 compounds on four common stationary phase columns used in GCwere given.Then separated experiments for two samples were made.It's satisfactory to select the optimal ratio of mixed stationary phase column with computer.
    Investigation on Polarography with Linearly Changing Potential (Ⅸ)——The Theory for Adsorptive- Complex Stripping Reversible Waves with CAEM Mechanism
    Gan Zhixing, Zong Huimin, Zhang Zuxun
    1989, 10(7):  696-699. 
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    In this paper the authors developed the theory of adsorptive- complex stripping reversible waves for linearly changing potential polarography on stationary hanging mercury electrode.According to the reaction schemethe(这里有图片19890705-696-1.gif) he equation is given by i=(n2F2/RT)·vA·[η/(1+η)2]DoCM{t2/r0+[2t21/2/(πDo)1/2]+2t11/2/[(3/7)πDo]1/2}Experiments with In3+-Cupferron complex in HOAc-NaOAc solution were carried out to verify he theory.The observed values agreed with the theoretical ones.
    Studies on Flow Injection Analysis-Electrochemical Detection System for Analyzing L-Lactate Dehydrogenase
    Zou Gongwei, Shi Jian, Chen Peihong
    1989, 10(7):  700-703. 
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    The new system for analyzing lactate dehydrogenase(LDH) by means of flow injection analysis-electrochemical detection has been established.The system was a single flow-way with a single pump.The PTFEreaction tube was 15 cm long(0.5 mmi.d.).The LDHcatalyzes the reaction between lactate and nicotinamideadenine dinucleotide(NAD).The nicotinamide adenine dinucleotide redused(NADH), which is product of above reaction, was determined by flow-cell amperometric detection.According to the kinetic curve obtained by spectrophotometry, the activity of LDHwas determined.The carrier was composed of 0.02 mol/L Na2HPO4, 0.4 mol/L NaNO3 and 0.06 mol/Llactic acid, the pHof the mixture was 9.4.The flow rate was 200 μL/min.The sample solution contained 1.015× 10-3 mol/L NAD, the sample volume injected was 10 μL.The working electrode was made of carbon paste and the potential was +0.80 V(vs SCE).
    Ridge Regression Estimation for Ill-conditioned Systems of Multicomponent Spectrophotometric Determination
    Liang Yizeng, Lu Zhiqiang, Yu Ruqin
    1989, 10(7):  704-708. 
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    The multicomponent spectrophotometric determination of the organic mixture system containing phenolic compounds was investigated.For these ill-conditioned systems with very similar spectral characteristics, both ordinary least squares regression and Kalman Filtering methods are not able to give satisfactory results.We used the ridge regression method newly developed in statistical literature to treat these ill-conditioned systems.The results obtained are evidently superior to those obtained by ordinary least squares or Kalman methods.
    Study on the Technique of ICP-AES by Using Electrothermal Graphite Furnace as Sample Introduction Device——Device and Its Analytical Performance
    Huang Min, Xu Lianfa, Jiang Zucheng, Zeng Yun'e
    1989, 10(7):  709-712. 
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    An instrument system is described in which a graphite furnace electrothermal vaporization device is used for the.introduction of microlitre liquid sample into an inductively coupled plasma.The appratus is equipped with home-made ones.Under the optimum operating condition for ICPexcitation and graphite furnace evaporation, the detection limits are at sub-nanogram level with linear dynamic ranges of over four orders of magnitude for nine elements.The RSDare better than 5%.
    Studies on the Reaction of 1,4-Dilithio-1,2,3,4-Tetraphenyl-1,3-Butadiene with Carbon Halide(Ⅱ)——Reaction with Methyl Bromide
    Huan Zhenwei, Liu Weiguo, Gao Zhenheng, Yao Xinkan, Wang Honggen
    1989, 10(7):  713-717. 
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    Cis, Cis(Ⅲ) and Cis, trans(Ⅳ) isomers of 2,3,4,5-tetraphenyl-2,4-hexandiene are obtained from the reaction of 1, 4-dilithio-1,2,3, 4-tetraphenyl-1, 3-butadiene (I) with methyl bromide.The reaction path is studied.The molecular structures and the ratio of the isomers were determined by MS, NMRand single crystal X-ray diffraction.1 belongs to the monoclinic, space group P2/n with the unit cell parameters of a= 6.567(3), 6=7.608(2), c=22.078(6)Å, β=94.29 (3) and Z=2.IVbelongs to the monoclinic, space group P21/c with the unit cell parameters of a = 12.256(2), 6=9.401(1), c=19.392(2)Å, β=99.35(1) and Z=4.Their final R-factors are 0.074 and 0.035 respectively.
    Studies on Nitroxides(XXIII) The Single Electron Transfer Reaction Between Piperidine Nitroxide, Its Oxoammonium salt and N.N.N',N'-Tetramethyl p.Phenylenediamine in Aqueous Solution
    Gao Zhongli, Zhang Fa, Liu Youcheng
    1989, 10(7):  718-723. 
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    The investigation by ESRspectroscopic and flow-stop kinetics UVmethods shows that in aqueous solution.
    Synthesis and Optical Properties of Some E, E-1,4-bis-[2',2"-(Benzoxazolylethenyl)]Benzene and Its Substituted Derivatives
    Zhou Yimin, Wu Yanmin, Gao Zhenheng
    1989, 10(7):  724-728. 
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    E,E-1,4-bis[2', 2"-(benzoxazolylethenyl)]benzene and thirteen of its substituted derivatives were synthesized.Their m.p., ultraviolet-visible absorption spectra and fluorescence emission spectra, fluorescence quantum yields as well as laser properties were determined.Configurations of these compounds were identified by IRand 1H NMR.The relationship between optical property and structure was discussed.It was found that E,E-1, 4-bis[2', 2"-(benzoxazolylethenyl)]benzeneand its substituted derivatives possess well photochemical stability and higher laser conversion efficiency than Coumarine-47.The synthesis of 2-methylbenzoxazole and substituted derivatives were also reported.
    Catalytic Characterization of the Dealuminized Faujusite ——Effect of the Nonframework Aluminiun
    Jiao Qingzhe, Jiang Dazhen, Fan Shuguang, Cao Jianhua
    1989, 10(7):  729-733. 
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    By hydrothermal treatment or silicon tetrachloride reaction at a high temperature, we have succeeded in reducing the content of Al atom in zeolite HYand obtained two series of deafuminized Yzeolite named as USY(W) containing nonframework Al and USY(T).USY(W) and USY(T) were characterized by TPD.IRand ESCA.The results shows that the nonframework Al in the USY (W) screens the strong acid sites of the surface and produces weak acid sites.The effects of Si/Al ratio and nonframework Al on the cumene- cracking activity of dealuminated zeolite were examined.The results shows that the higher the Si/Al is, the smaller the catalytic activity is.Besides, the nonframework Al in the USY(W) exerts a influence on the catalytic activity of zeolite in cumene-cracking and coking.The catalytic activity of zeolite decreases with the formation of non-framework Al and the coking amount reduces obviously.
    Structural Rule of Borane Cluster Compouds
    Wang Rongshun, Zhang Xiaohui, Zhang Jingping
    1989, 10(7):  734-737. 
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    The structures of borane cluster compounds were discussed.The structural rule of dense borane were advanced based on the number of above electron, we discussed the relationships of some structural rule of borane cluster compounds.
    A Study on Ion Pair and Ionic Solvation of Ca(ClO4)2 in Some Solvents and Their Mixtures by 35Cl NMR
    Li Zhifen, Qian Hong, Huang Yining, Liu Ruilin
    1989, 10(7):  738-742. 
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    This research has recorded the linewidth of 35Cl of 0.5 mol/L Ca(ClO4)2 solution in ten solvents and the variation of linewidth with concentration of salt in six solvents.The relation between ionic association and the properties of solvent and ion was explored.The linewidth of 35Cl in acetoni-trile or ethanol as bulk solvent at fixed concentration of Ca(ClO4)2 was measured as a function of [B]/[Ca2+], where Brepresents H2Oor DMF.The trend of the plot and the reason for that were explained.The solvation numbers of Ca2+ by solvents were withdrawn from plots.The type of ion pairing of Ca2+ and ClO4- was assumed based on the conductance data.
    Studies on the Cyclic Voltammetric Behaviour of the Prussian Blue Film Modified Electrode
    Liu Biao, Hui Teng'en
    1989, 10(7):  743-746. 
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    The cyclic voltammetric studies on the Prussian Blue(PB) film modified electrode are reported.It is shown that the interaction among the electroactive centres in the PBfilm leads to the difference of the voltammetric behaviour of the modified electrode from ideal waves.For the high scanning rate, the voltammetric behaviour can be explained in terms of the finite diffusion interface model.In a- solution containing potassium ions the charge transport diffusion coefficients are found to be 10-9-10-11cm2/s.
    Studies on the Adsorption and Separation Capacity of the New Resins (AAS) for Phenylalanine and Tyrosine
    Wang Shouting, WangBusen, Guo Zhenliang, Wang Chunlai, He Binglin
    1989, 10(7):  747-752. 
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    The adsorption and separation capacity of the new resins AASfor phenylalanine and tyro-sine was studied.The relationship between the structure of the resins and the adsorption and separation capacity was analysed.The separation mechanism of the chromatography was also investigated.
    Balloon and Liquid Adhesion Effect in Dynamic Membrane Osmometry Determination
    Shao Yufang, Hong Huaimao, Cheng Rongshi
    1989, 10(7):  753-756. 
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    The influences of the balloon effect, i.e.the elastic deformation of the semipermeable membrane and the adhesion of liquids on the capillary, wall, on the measurement of solvent permeation rate and osmotic pressure of polymer solution were investigated by dynamic method theoretically and experimentally.The balloon effect leads to the departure from linearity of the plot of permeation rate of solvent against the hydrbstatic pressure difference.This effect could be described quantitatively by a deformation factor which is closely related with swelling ratio of the membrane in the solvent.The adhesion of liquids on the capillary wall influences the reproducibility of measurements and is the main reason for the occurrence of the unsymmetry of ascending and descending lines.
    Synthesis and Characterization of N,N'-Dimethyltriglycodianilide and Its Complexes with Rare Earth Nitrates
    Jiao Tianquan, Can Xinmin, Tan Minyu, Tang Ning, Lei Runzhi
    1989, 10(7):  757-759. 
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    Anew open-chain crown ether,N,N'-dimethyltriglycodianilide,and its complexes with rare earth nitrates were synthesized.These complexes were characterized by elemental analyses,IRspectra, NMRspectra and molar conductance.
    Alkali Metal Ion Selectivities for BLM Modified by Bis-Crown Ethers
    Tai Zihou, Wang Defen, Sun Xiaoqiang, H. Ti. Tien
    1989, 10(7):  760-762. 
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    Astudy of the monovalent cation transport through BLMmodified by five kinds of bis-crown ethers using electrochemical measurements is presented.An investigation of the BLMpotential, ion selectivities and current on the membrane has been carried out and the experimental results indicated that using BLMwe can compare the selcctivities for some monovalent cations of various bis-crown ethers which have similar molecular structure and chemical properties.
    Effects of Concentrations of Reagents on Polymerization Reaction of Aluminosilicate
    Li Shougui, Xu Ruren
    1989, 10(7):  763-765. 
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    Effects of concentration of reagents on polymerization reaction of aluminosilicate were investigated.The polymerization reaction is accelerated as the concentration of Al2O3 increases and is slowed down as the alkalinity or concentration of potassium increases.The influence of the concentration of SiO2 is complex.Under the condition of a high silica/alumina ratio the rate of polymerization decreases with increasing concentration of SiO2, but under the condition of a low silica/alumina the rate of polymerization increases with increasing concentration of SiO2.
    Synthesis of 3-Carbethoxy-2-Methyl Quinoline Derivatives
    Ju Benzhi, Jiang Guiji, Gao Yongjun
    1989, 10(7):  766-768. 
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    Compounds (2)-(4) were synthesized through condensation of 3-carbethoxy-2-methyl quinoline with ester and cyanides, respectively.Compound (5) was obtained from direct hydrolysis of (1) in the presence of alkalis.Compounds (10)--(13) were produced by cyanoethylation, condensation, acetylation and methylation of the compound (9),respectively.The structure of these ten com pounds were confirmed via elemental analysis, IRand 1H NMR.
    Catalysis of New Type Acyclic Polyether Amine in N-Alkylation of Benzotriazole
    Hu Aixi, Zeng Zhaoqiong
    1989, 10(7):  769-771. 
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    Effects of polyethylene glycols, quaternary ammonium salt and acyclic polyether amine on the yields of N-alkylation of benzotriazolc in liquid-liquid phases were examined.Selecting better a-cyclic polyether aminc as phase transfer catalyst, alkylhalids as alkylating agents, we have synthesized seven N-alkyl benzotriazoles.The results show that acyclic polyether amine is good liquid-liquid phase transfer catalyst and the yields of the N-alkylated products are high.
    Molecular and Crystal Structures of Involucratolactone
    Wang Qiguang, Li Yu, Jia Zhongjian
    1989, 10(7):  772-774. 
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    Involucratolactone, C21H30O8, Mw=410.47 is monoclinic, and its space group and lattice parameters are as follows; P21, a=22.195(3)Å, b=6.584(1)Å,c=20.728(4)Å, β=98.32 (1)°, V= 2997.9(9)Å3, Z=6, Dc=1.365 g·cm-1, μ(CuKa) = 11.02 cm-1.The crystal structure analysis shows that it is a new sesquiterpenoid glycoside.
    The Standard Electrode Potential of Standard Zinc Amalgam Electrode at 298 K
    Hui Yongji
    1989, 10(7):  772-777. 
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    This paper reports the determination of the electrode potential of six different concentrations zinc amalgam (varies from 0.00050 to 0.3472 mol/kg) in a saturated ZnSO4 solution.Two reference electrodes were used during the measurement.The result of the potential measurement for each Zn amalgam electrode agrees to be with ± 5μV.
    A New Method for Solid Acid-Base Strength Distribution Measurement
    Xu Zheng, Qian Zaihu, Cui Shengfan
    1989, 10(7):  778-780. 
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    Anew method for solid acid-base strength distribution measurement is suggested.We used CO2 as the adsorption gas for determining base strength distribution and NH3 as the adsorption gas for determining acid strength distribution.We suggest that we can use,△H/Tto represent the acid and base strengthes, and the amounts of adsorbed gases to represent the acidity and basicity.The results obtained by this new method are almost the same as that of the titration method using Hammett indeca-tor.This method can be used not only for calorless catalysts but also for calorful catalysts without using any solvent.We can also inspect the acid-basic qualities of industrial catalysts at the condition close to that catalytic reaction.
    Studies on Shrinkage-Compensation Effect of Unsaturated Polyester (Ⅰ) ——Shrinkage-Compensation Effect of Several Common Polymers
    Gao Shanjuan, Wu Xuemei
    1989, 10(7):  781-783. 
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    The shrinkage- compensation effects of five polymers such as PS, PE, PVC, 330* polyether, alkyd resin on 191* unsaturated polyester were examined.These polymers were used in the preparation of low-profile sheet-molding and bulk-molding compounds and the mechanical and thermal properties of these products were also determined.The properties of these modified unsaturated polyesters are satisfactory.
    Polymer-Supported Stannic Tetrachloride Complex Catalysts (Ⅱ)——Copolymer (Styrene-Methyl Methacrylate)-Stannic Tetrachloride Complex
    Ran Ruicheng, Mao Guoping
    1989, 10(7):  784-786. 
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    Across-linked polymer carrier beads, styrene-methyl methacrylate(19%)-divinylbenzene (2%) copoiymer, were synthesized and combined with stannic chloride in chloroform to form a stable complex containing 20.5% Cl (equivalent to 1.44 mmol SnCl4/g of complex beads).The complex showed a good catalytic activity for many organic reactions such as esterif ication, ketal formation, and etherification.The catalyst can be used for six times at least without losing its catalytic activity.
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