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    24 April 1990, Volume 11 Issue 4
    Articles
    Studies on the Structure and Properties of Divalent Metal Aluminophosphate Molecular Sieve
    Han Shuyun, Yang Chuncai, Wei Quan, Yuan Hanzhen
    1990, 11(4):  331-335. 
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    The pure MeAPO-5 type molecular sieve was synthesized [Me=Mg( Ⅱ ), Fe( Ⅱ ,Ⅲ ), Co ( Ⅱ ), Ni(Ⅱ ), Zn( Ⅱ ), Mn( Ⅱ )] by hydrothermal method. Their ability of adsorption, thermal stability and structure were also investigated by means of XRD, IR, XPS, ESR, Mossbauer, electron probe and MAS NMR. The results show that the structure of MeAPO-5 molecular sieve are AlPO4-5 type and Metal atom enters the framework of MeAPO-5 molecular sieve.
    The Liquid-Liquid and Liquid-Solid Extraction System of Polyvinyl Pyrrodidone- (NH4)2SO4-H2O
    Li Buhai, Wang Kefu
    1990, 11(4):  336-339. 
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    The aqueous solution of polyvinyl pyrrodidone can be separated into two liquid or a liquid and a solid phases in the presence of (NH4)2SO4. The conditions of phase separation were found. The distribution behaviour of water-soluble ligands and their metal chelates between the two phases were investigated. The quantitative extraction separation of Zr(Ⅳ )-La( Ⅲ ) was carried out. The extraction machanism for PVPphases was also studied.
    Syntheses of Rare Earth Molybdoarsenate Heteropoly Complexes and Their Properties
    Wang Enbo, Hu Changwen, Zhou Yanxiu, Liu Jingfu
    1990, 11(4):  340-344. 
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    In this paper, the preparation of heteropoly compounds (NH4)17(RE(Assub>2Mosub>17O61)2) · nH2O (RE=La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Yb, Y) is reported. The physical and chemical characters of the new preparative heteropoly compounds were studied by using UV, IR, CV, TG-DTApolarography. It was determined that the condition under which the heteropoly anion RE (Assub>2Mosub>17O61)217- could stably exist in solution is pH=2.8-4.0 at room temperature. The redox properties of rare earth molybdoarsenate complexes in solution and their thermal stabilities were also studied. It was deduced that heteropoly compounds (NH4)17[RE(As2Mo17O61)2] · nH2Oand K16[Ce(a2-P2W17O61)2] · 50H2Ohave the same structure.
    Studies on the Synthesis and Characterization and Bonding Specificity of Rare Earth ( Ⅲ) Complexes with Indole-3-Acetic Acid and Indole-3-butanoic Acid
    Wang Zemin, Fu Chujin, Cao Jinrong, Lu Feng
    1990, 11(4):  345-349. 
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    Eight new solid complexes of rare earth ( Ⅲ ) with indole-3-butanoicacid and indole-3-bu-tanoic acid were synthesized in ethanol-water soluton. The new complexes have the composition Ln (IA)3·2H2Oand Ln(IB)3·2H2O(Ln = La,Nd,Sm,Er,IA = C10H8NO2, IB = C12H12NO2). The electronic spectra of the complexes were observed. The molar conductance data show that the complexes are non-electrolyte. IRspectra and XPSmeasurements indicate the unidentate coordination mode of carboxylate ions to rare earth (Ⅲ ) ion in Ln(IA)3 · 2H2Ocompounds and the bidentate coordination mode of carboxylate ions in Ln(IB)3 · 2H2Ocompounds, also show that nitrogen atoms in indole-3-acetates are coordinated, but nitrogen atoms in indole-3-butanoates are uncoordinated. The TG-DTAdata show that the complexes are all relatively stable thermally.
    Sensitivity of Synchronous Scanning-Derivative Fluorimetry
    Xu Jingou, Xu Ruitong
    1990, 11(4):  350-354. 
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    Amodified empirical equation (Eq. 1) for the calculation of the peak half-width of the synchronous fluorescence band and a calculation equation (Eq. 2) of the peak height of the derivative spectra were presented in order to explain that the sensitivity of synchronous scanning-derivative fluorime-try is higher than those of conventional, synchronous and derivative fluorimetry theoretically.
    A Study on Extraction Chromatographic Separation of Tungsten and Molybdenum with TOPO
    Liu Shaoling, Wen Jingwei
    1990, 11(4):  355-358. 
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    The behaviour for extracting Wand Mo from HC1 solution with TOPOin xylene was studied. Based on this, an extraction chromatographic method is proposed for separation of Wand Mo by using GDX-103 resin as the support and TOPO-xylene as the stationary phase. After eluting coexistent ions with 4 mol/L HC1-0. 05 mol/Ltartaric acid, Wand Mo are separated by elution with 1 mol/L HC1-0. 05 mol/Ltartaric acid and 0. 01 mol/Ltartaric acid. The method combined with SAF-CTMABspectrophotometry has been applied to determining Wand Mo in alloy steels and geochemical samples with satisfactory results.
    Investigations on Polarography with Linearly Changing Potential (Ⅺ) —The Adsorptive-Complex Wave of Cu( Ⅱ )-Histidine
    Wu Zhibin, Zhang Zuxun
    1990, 11(4):  359-362. 
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    In this paper, the polarographic behaviors of Cu ( Ⅱ )-histidine adsorptive-complex wave have been studied in 0.2 mol/L NaOHmedium. The experimental results show that it is a irreversible wave. The composition, conditional stability constant(K) and dissociation constant(Kb) of the complex were determined. The mechanism of electrod process has also been discussed.
    Studies on the Adsorptive Stripping Catalytic System of Vanadium ( Ⅴ )
    Xu Hongding, Yu Guirong, Hu Gaosheng, Zhang Zhan'en
    1990, 11(4):  363-366. 
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    An adsorptive stripping catalytic system of vanadium ( V ) is studied in this paper. Abase solution consists of 1 × 10-5 mol/Lpyrogallol carboxylic acid(HL) and 0. 05 mol/L NaBrO3 in 0. 05 mol/L HAc-NaAc buffer (pH = 5). In this base solution, the complex HVO3L22- was adsorbed onto the DMEat - 0. 15 V(vs SCE). An adsorptive stripping catalytic wave appeared when the electrode potential was scanned to - 0. 9 V. Peak potential was at - 0. 7 Vor so. The peak current was very sensitive. The detection limit of vanadium ( V ) is 6×10-13 mol/L. Using this system for analysis of samples such as natural water, liquor and hair, satisfactory results were obtained.
    A Study on the Thin-Layer Chromatography and Ultraviolet Spectrum of Dicyclo-pentadienyl Ytterbium and Dysprosium o-Substitutied Benzole Acid Derivatives
    Li Songlan, Yang Xuejin, Sun Cheng, Liang Shusen, Ye Zhongwen
    1990, 11(4):  367-370. 
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    The thin-layer chromatography behavior of dicyclopentadienyl ytterbium and dysprosium o-substituted benzoic acid derivatives is studied using silica gel Gplate impregnated with decane. The following rules have been obtained:1. The Rf values are decreased as the increasing of the electron donating ability of o-substituting group in the aromatic ring.2. The silica gel plate impregnated with decane diminishes the absorbing activity only, but has no effect on the behavior of absorption chromatography.3. The Rf values change in the opposite direction with the λmax, values of ultraviolet spectrum for the series of compounds. The preliminary discussion is also made for this relationship in theory.
    Regiosclective Cycloaddition Reaction of (Z)-1 ,2-Diphcnyl-1,3-butadiene with Monosubstituted Ethylenes
    Xie Zhou, Xu Xiangong
    1990, 11(4):  371-375. 
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    The cycloaddition reactions of (Z)-J ,2-diphenyl-1, 3-butadiene were studied with a high regioselectivity. The products were identified by IR, NMRand MS. The regioselectivity in the Diels-Alder reactions of (Z)-1 ,2-diphenyl-1,3-butadiene can be rationalized by frontier orbital theory. The primary orbital interactions which have been used to predict the regioselectivity in the Diels-Alder reaction could not account for the regioselectivity observed with (Z)-1,2-diphenyl-1,3-butadiene. When the secondary orbital interactions were included in the theory, the preferred regioisomer was rationalized in every case. The frontier molecular orbitals of (Z)-1, 2-diphenyl-1, 3-butadiene and the dienophiles were determined by the CNDO/2 method.
    Study on Intramolecular Hydrogen-Bonding and Keto-Enol Tautomerism of Some Asymmetrical β-Diketones by1H NMR
    Zhang Benli, Zhuo Jincong, Gui Mingde, Gao Zhenheng
    1990, 11(4):  376-379. 
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    The intramolecular hydrogen-bonding and keto-enol tautomerism of a series of 1-aryl-3-tolyl-1,3-propanediones were studied by 1H NMR. Both δOHand lgK(K=[enol]/[keto]) can be correlated with substituent constants satisfactorily. +1 and +Rsubstituents enhance the hydrogenbond-ing and decrease the content of enol form.
    Alkylation of Isobutane with Butenes on H3PO4-BF3/ZrO2及H3PO4-BF3H2SO4/ZrO2
    Qian Zaihu, Liao Shijun
    1990, 11(4):  380-384. 
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    Anew type of alkylation catalysts for isobutane with butenes were prepared by ZrO2 impregnated with H3PO4-BF3or H3PO4-BF3-H2SO4 and dried at lower temperature. The effects of the calcination temperature of ZrO2, the concentration of impregnation solution, the addition of BF3 and H2SO4, and the reaction temperature on the activity of catalysts were researched. Acidity and stability of these catalysts were also discussed.
    Studies on Fluorescence Enhancement Effect of Eu-Gd-DBM-NH3- Organic Solvent System
    Yang Jinghe, Zhu Guiyun, Si Zhikun, Wang Dafang
    1990, 11(4):  385-388. 
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    In the present paper, solvent and co-luminescence effects of Eu-DBM-NH3 system are reported. The results show that the organic solvents (such as methanol, acetone, ethanol) make the system to produce sensitized fluorescence considerably.Anew fluorescence-enhanced phenomenon, which is produced by adding Gd3+, Y3+, Tb3+, La3+ and Lu3+ to Eu-DBM-NH3-acetone system, can be observed. Of these, Gd3+can enhance the fluorescence intensity by two orders of magnitude in comparison with that of the system without Gd3+. Eu-Gd-DBM-NH3--acetone system can be used for the determination of trace amount of Eu3+ in the range from 1. 0× 10-10 to 6. 0×10-8 mol/L. The detection limit is 3. 0× 10-11 mol/L.In addition, the luminescence mechanism of this system is discussed.
    Studies on Vapor Liquid Equilibria Under Pressure for Benzene-n-Heptane-Ethanol Ternary System
    Wang Qi, Chen Genghua, Han Shijun
    1990, 11(4):  389-393. 
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    The vapor liquid equilibrium (VLE) data of benzene-n-heptane-ethanol ternary system under pressure of 101. 3, 302. 5, 506. 8, 709. 3, 810. 6 kPa were determined with the double circulating VLEdevice under pressure. The ternary VLEdata were predicted with multicomponent Wilson equation, and the energy paired parameters were obtained from the correlation of VLEfor three binary systems i. e. benzene-n-heptane, benzene-ethanol, n-heptane-ethanol under corresponding pressure. The good agreements between predicted values and experimental data were obtained.
    Studies on Electrochemical Behavior of Infield Emissive Electrode
    Zhang Linshao, Pan Yanwang, Shun Bingyin, Wang Jun, Jiang Dapeng
    1990, 11(4):  394-396. 
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    In this paper studies some electrochemical behavior of infield emissive electrode which is made from N-Si and P-Si semiconductor with chemical precipitation method. The decomposition potential i-Kcurve indicates that this electrode can decompose water below 1. 23 Vand the cyclic voltam-mogran of Fe3+/Fe2+ system indicates that the peak electric current of this electrode is eight times higher than that of platinum electrode.
    Synthesis and Studies on the Non-Isothermal Kinetics of Thermal Decomposition of La(NCS)3·3TMSO2
    Suo Zhanghuai, Sun Tongshan, Jiang Bengao, Yin Jingzhi
    1990, 11(4):  397-401. 
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    The complex of lanthanum isothiocynate with sulfolane was synthesized. The kinetics of thermal decomposition of the complex was studied under non-isothermal condition. The non-isothermal kinetic data were analyzed by means of the Achar method and the Coats-Redfern method. The possible reaction mechanism was suggested by comparison of the kinetic parameteres. The results show that this thermal decomposition is a second order reaction. The kinetic equation may be expressed as :da/dt = AeE/RT · (1 - a)2.Mathematical expression of the kinetic compensation effect is found to be:InA = 0.218E - 0.637.
    The Microphase Separation and Surface Proparty of Graft Gopolymers Prepared by Polystyrene Macromer and Butyl Acrylate
    Ma Keqin, Hu Chunpu, Wang Shirong, Wu Shusen, Ying Shengkang
    1990, 11(4):  402-405. 
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    By using "macromer technique", the well-defined graft copolymers with polystyrene (PS) as side chains and polybutyl acrylate (PBA) as backbones were prepared and the microphase separation as well as the surface property of these graft copolymers were studied. The experimental results showed that the partial microphase separation could not be observed until the number average molecular weight of the PSside chain was more than5900 and the critical surface tension γc was not affected obviously by the composition and the microphase separation of those graft copolymers, but affected by the polar liquid series used (ethanol/water and ethylene glycol/n-octanol). However, the values of γSD (dispersion energy of those copolymer surfaces) calculated by the Good-Giraflco-Fowkes-Young equation were almost constant for all polymers studied here. The results also showed that both sides of the graft copolymer film surfaces were enriched with PBAbackbone.
    Studies on the Polysilanes ConMning Four Membered Rings with Si-N Bonds in the Backbone
    Du Zuodong, Wang Qin, Chen Jianhua
    1990, 11(4):  406-409. 
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    Polysilanes containing four membered rings with Si-Nbonds in the backbone were synthesized by cocondensation of methyl (β- phenethyl) dichlorosilane (or diphenyldichlorosilane ) and N,N'-bis-(chlorodimethylsilyl)tetramethylcylclodisilazane with sodium metal in toluene. The polymers possess higher molecular weights, lower softening points, better solubilities in common solvents. By casting the solution of each of the polymers in toluene on a glass plate, an elastic transparent film with fairly mechanical strength can be obtained. The polymers with some electron acceptors, such as(这里有图片19900418-406-1.gif)etc., can form C. T. complexes which show strong UVabsorption bands at a relatively low energy.
    Studies on Thermal and Dynamic Mechanical Properties of RIM and Solution Polymerized Polyureas with Various Hard Block Contents
    Chen Zhusheng, Willkomm W R, Macosko C W
    1990, 11(4):  410-413. 
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    Aseries of amine terminated polypropylene oxide based on thermoplastics polyureas with 30%,50% ,and 70% hard segment contents were synthesized via solution polymerization and reaction injection moulding (RIM). Amine terminated polypropylene oxide was used as the soft segment and 4,4'-diphenylmethanediisocyanate (MDI) extended with diethyltoluenediamine (DETDA) was used as the hard segment. These polyureas were characterized by differential scanning calorimetry (DSC), dynamic mechanical spectroscopoy (DMS). RIMpolyureaas have poorer phase separation than solution polyurea as seen by DSC,DMS, especially at high hard segment levels. Any evidence of a hard segment glass transition in polyureas has not been found by DSCand DMS.
    Studies on Voltammetry Determinatibn of Trace Amount of Gold by Tri-n-Octylamine Modified Electrode
    Shi Qingzhao, Hong Jianjun, Lu Rongshan, Ma Guoqiang, Zhou Ying
    1990, 11(4):  414-416. 
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    The determination of trace amount gold( Ⅲ ) with tri-n-octylamine as the modified glassy carbon electrode in1.5 mol/Lhydrochloric acid medium by cathodic voltammetry is presented. Ahighly sensitive irreversible reduction peak was obtained at potential +0. 16V(vs SCE). Alinear relationship between the peak height and concentration in the range of 5× 10-7-5× 10-9 mol/Lof gold was observed. The detection limit was found to be about 0.1 μg/mL (3-min preconcentration). This method is applied to measure the trace amount of gold in anode mud and the results are satisfied, with the coefficient of variation 6.42%(at 26 ppb level) and the percentage of recovery 95%-101 %.
    Oscillo-Potentiometric Titration of Berberine Hydrochioride
    Hu Xiaoya, Leng Zongzhou
    1990, 11(4):  417-419. 
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    The copper plate coated with PVCmembrane (containning berberine-tetraphenylborate) was used as the indicator electrode, while berberine was titrated with sodium tetraphenylborate by oscillo-potentiometric titration. This method is precise, audio-visual, simple and convenient and can be used in the determination of other drugs.
    The Behavior of Reimer-Tiemann Reaction Under the Catalysis of PEG
    Kang Ruhong, Zhang Xiuli, Li Guoping, Zhang Lanping
    1990, 11(4):  420-422. 
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    Reimer-Tiemann reaction under phase transfer catalysis of poly (ethylene glycols) (PEG) has been studied. It has been shown that PEGhave an obvious catalytic effect on the reaciton and the ratio of the para- and ortho-products is abnormal. Such an abnormal Reimer-Tiemann reaction has not been reported in literature. The conditions of the abnormal Reimer-Tiemann reaction were studied in detail and a mechanism was proposed.
    A New Triterpenoid form Kadsllra Heteroclita (Roxb)Craib
    Dai Ping, Han Guiqiu
    1990, 11(4):  423-424. 
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    Anew triterpenoid, named iso-anwuweizic acid, was isolated from the roots of Kadsura hete-roclita(Roxb)Craib. Its structure was elucidated as 3a-hydroxy-lanost-9(11), 21-dien-26-oic acid by means of UV, CD, IR, MS, 1H NMR, 13C NMRand 2D-COSY NMR.
    Chemistry of 1,2,4-Triazines(XIV)—Synthesis of 3-Methoxy-5-Methyl-6-Acetyl-1,2,4-Triazine and Its Condensation with Aromatic Aldehydes
    Cheng Tieming, Lei Guangqing, Wang Laixin, Wang Dong, Cai Mengshen
    1990, 11(4):  425-427. 
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    3-Methoxy-5-methyl-6-acetyl- 1, 2, 4-triazine ( Ⅱ ) was synthesized and condensed with aromatic aldehydes to give 3-methoxy-5-methy]-6-(4-hydroxy)-cinnamy)-] ,2. 4-triazine( Ⅲ ) or 3-methoxy-6-acetyl-5-(2-aryl)-vinyl- 1, 2, 4-triazines ( Ⅳ ). The structure of these products were proved by IR, UV, MS, 1Hand 13C NMRspectra.
    A New Route for the Synthesis of the Main Component of San Jose Scale's Sex Pheromone
    Wang Shimin, Xu ZHanghuang
    1990, 11(4):  428-430. 
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    Anew method for the synthesis and monoprotection of 2,6-heptanedione(2) is reported. 3, 7-Dimethyl-2,7-octadien-l- yl propanoate (1), the main component of San Jose Scale's sex pheromone, was synthesized by a two-step Wittig reaction from 6-(1,3-dioxolan-2-yl)-2-heptanone (3) in 31% yield. Z : E=19 : 81. The total yield is 11%.
    Studies on Electrochemical Polymerization of Acetylene
    Huan Zhengwei, Qiao Yinan, Yang Guang, Shen Zhiquan, Hu Shizhao, Zhou Xiaoxia
    1990, 11(4):  431-433. 
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    Fe-doped polyacetylene film was prepared successfully on a stainless steel cathode by gal-vanostatic polymerization method at room temperature in Fe(NO3)3·9H2O-DMFsolution. The various factors affecting the polymerization process were investigated. Instrumental analyses show that the configuration of the film is mainly trans-(CH)z doped with Fe ca. 10% and the morphology of the film is polycrystals with a net texture.
    The Preparation and FTIR Spectra of LB Monomolecular Films
    Xu Weiqing, Tian Yongchi, Zhang Danzhe, Liang Yingqiu
    1990, 11(4):  434-436. 
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    LBmonomolecular films of octadecanoic acid were prepared to the surface of a CaF2 plate by home-built apparatus, and the FTIRtransmission and ATRspectra of the LBfilms were recorded.
    Thermodynamics of Rare Earth ( Ⅲ )-Crown Coordination Reaction
    Liu Deqian, Jiang Bengao, Yin Jingzhi, Yan Haike
    1990, 11(4):  437-439. 
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    The coordination reaction of lanthanum and ytterbium perchlorates with dibenzo-30-crown-10 in acetonitrile was determined at 298. 15 Kby calorimetric titration. The reaction enthalpies were calculated by using computer. The results show that the enthalpy changes are exothermic.
    The Kinetic Study on the Copolymerization of Butadiene with Styrene Catalyzed by Co(nap)2-Al2Et3Cl3 System
    Li Zhu, Hu Liping, Jiao Shuke
    1990, 11(4):  440-441. 
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    The kinetic study on the copolymerization of butadiene with styrene catalyzed by the binary system Co(nap)2-Alsub>2Etsub>3Clsub>3 was carried out. The dependence of reaction rate on the polymerization conditions, including the concentration of catalyst and monomer and the temperature of the reaction were investigated. The rate constant and the apparent activation energy were obtained.