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    24 October 1999, Volume 20 Issue 10
    Articles
    Synthesis and Characterization of H-form Aluminosilicate MCM-41 in a Novel Alkali-metal Free Media
    LIN Wen-Yong, PANG Wen-Qin, WEI Chang-Ping, LI Dong-Mei, ZHEN Kai-Ji
    1999, 20(10):  1495-1498. 
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    Incorporation of aluminum into MCM-41 framework was achieved in an alkali-free system, by using diethylamine as the base source. The properties of the product are compared with those of the samples obtained with NaOH. XRD and TEM results show that the resulted materiaLIs highly ordered. 27AlMAS NMR experiment indicates that aluminum atoms are present with a 4-coordinated form in the as-synthesized samples. Upon calcination, a small amount of Al was removed from the framework, as indicated by a small peak characteristic of 6-coordinated ALIN the NMR profile. The surface acidity of the calcined samples were studied with Py-IR technique.
    A Study of the Isothermal Solubility of Ternary Systems CuSO4(ZnSO4)-CO(NH2)2-H2O at 30 ℃
    ZHANG Feng-Xing, ZHAO Pei, YANG Qin, GUO Li-Juan, SHI Qi-Zhen
    1999, 20(10):  1499-1503. 
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    CuSO4-CO(NH2)2-H2Oand ZnSO4-CO(NH2)2-H2O ternary systems have been in-vestigated by isothermal method at 30 ℃. Their solubility diagrams and refractive index-composition diagrams have been constructed. New ternary compounds formed in each system respectively, CuSO4·3CO(NH2)2·H2Oincongruently dissolved in the former system and ZnSO4·CO(NH2)2·2H2O congruently dissolved in the latter and new compounds were confirmed by IR, TG and X-ray diffraction methods.
    Syntheses, Crystal Structure and Spectra of Mixed Ligand Complex of Lanthanide [Ln(BA)2(NO3)(phen)]2
    XIAN Chun-Ying, ZHU Long-Guan, YU Qing-Sen
    1999, 20(10):  1504-1508. 
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    New mixed-ligand complexes of lanthanides [Ln(BA)2(NO3)(phen)]2(BA=ben-zoate, phen=1,10-phenanthroline) have been synthesized in aqueous solution of slight acidity and characterized by elementary analysis, IR and DTA-TG. Their ESR and fluorescence spectra were studied. The result of the crystal structure of Pr-complex shows that the complex is triclinic, space group P1, a=1.1007(8)nm, b=1.1177(3)nm, c=1.0687(4)nm, α=98.10(3)°, β=110.62(4)°, γ=84.80(4)°, Z=1, V=1.217(1) nm3, Dc=1.706 g/cm3, F(000)=620.00, μ(MoKα)=20.47cm-1. The crystaLIs consisted of a binuclear molecule. The coordination number of Pr3+is nine. The four BA ligands have two coordination modes: bidentate bridging and tridentate bridging.
    Synthesis, Characterization and Molecular Recognition of meso-Tetrakis(o-BocGlyamidophenyl)porphyrinatozinc
    WANG Chuan-Zhong, ZHU Zhi-Ang, RUAN Wen-Juan, LI Ying, YAN Shi-Kai, CHEN Rong-Ti
    1999, 20(10):  1509-1514. 
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    meso-Tetrakis(o-BocGlyamido)porphyrin[H2T(o-BocGly)APP),1] and its zinc complex [ZnT(o-BocGly)APP, 2] were synthesized and characterized. By means of spec-trophotometer technique, the equilibrium constants of the axial coordination reaction were measured between complex 2 and a series of imidazoles, molecular recognition of imidazoles by the receptor porphyrin 2 was studied. The results show that the equilibrium constants de-crease in the orders of K(Im)> K(2-CH3Im)> K(EMIm)> K(2-HOCH2Im) and K (Im)> K(N-CH3Im)> K(GMZ), suggesting that the steric effect was the key factor, the data of steric effect were calculated, the thermodynamic parameters (这里有图片19991004-1514-2.gif) and Δ r S ○? ? m were investigated by van′t Hoff′s equation, the phenomenon of enthalpy-entropy compensation was the observed in the coordination process.
    SAM Fabrication and Photoelectric Conversion Property of Two Pyrrolidinofullerene Carboxylic Acid Derivatives
    WEI Tian-Xin, ZHAI Jin, GE Jin-Hao, GAN Liang-Bing, HUANG Chun-Hui
    1999, 20(10):  1515-1519. 
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    The self-assembled monolayers of two pyrrolidinofullerene carboxylic acid deriva-tives on hydrophilic indium-tin-oxide(ITO) are fabricated. The SAMs were characterized by contact angle, UVspectrum, cyclic voltammetry. The photoelectric conversion properties of both compounds in SAMs and the effect of light intensity, bias voltage and electron acceptor on the photocurrent generation were studied.
    The Effect of Lamellar Liquid Crystals System on SOD-like Activity of Copper-Salicylate Complex
    XU Ke-Wei, GAO Yue-Ying
    1999, 20(10):  1520-1522. 
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    Copper-Salicylate complex was synthesized and its ability that inhibits the reduc-tion of NBT by the superoxide radical(O2·-) was measured in aqueous solution and in AOT, TX-100, CTAB lamellar liquid crystals systems. It is obtained that the copper complex had SOD-like activity either in solution(ID 50=1.1×10-6mol/L) or in AOT lamellar liquid crystal(ID50=2.0×10-5mol/L). Experiments show that AOT lamellar liquid crystal had SOD-like activity itself. The synergism of copper complex and AOT lamellar liquid crystal can enhance the SOD-like activity of the system.
    Artificial Olfactory Analyses of Micro-and Simple-Component Vapors
    GAO Da-Qi
    1999, 20(10):  1523-1527. 
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    Acascade neural network with radial basis function(RBF) and linear basis function(LBF) is proposed, and an artificial olfactory system made up of fourteen of SnO2model semiconductor sensors and a cascade neural-network classification method set up. Measure-ments and analyses for eight kinds of micro-and simple-methanol vapors as well as ethanol and acetone ones show that with the help of the presented method an artificial olfactory system has its performances such as sensitivity and discriminating ability greatly developed, that it is able to real time detect simple-component odors and multi-component ones. This development lays down a foundation for such a system to determine qualities of food fragrances.
    Development and Application of Chromatographic Gray Model(Ⅳ)--Establishment of CGM(1,1, N) Model and Prediction of Retention Behavior of Isomeric Alkylbenzenes
    ZHANG Su-Ping, SUN Zhao-Lin, ZHANG Xiao-Tong, LENG Jing, CAI Yang-Yong
    1999, 20(10):  1528-1532. 
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    We derived the N-parameter gray model--CGM(1,1, N) based on gray system theory in this paper. The complicated relationships between chromatographic retention be-havior of isomeric alkylbenzenes and molecular structure parameters have been successfully investigated using the gray model. The retention and the logarithm of the partition coefficient of isomeric alkylbenzenes have been predicted. The precision is higher than that of the single parameter model--continuous gray model CGM(1,1). CGM(1,1, N) is a practical method for the prediction of the retention behavior of solutes.
    Capillary Electrophoresis of Proteins Under the Control of Radial Electric Field
    ZHU Ying, CHEN Yi
    1999, 20(10):  1533-1537. 
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    Separation of basic proteins was performed using a homemade electric field modu-lated capillary electrophoretic system, which can offer both radial and axial electric fields with only one high voltage power supply. The most interesting phenomenon observed is that the adsorption of protein molecules onto the tubing wall can be regulated by the application of a radial voltage(potential at the outer wall minus that at the inner wall): band broadening decreases with the increase of the radial voltage. This implies that it may be possible to dy-namically control the adsorption of protein molecules on silica surface. In addition, the radial voltage is also able to adjust the resolution of the solutes due to the change of electroosmosis.
    Studies on Separation of Different Species Containing Boron in Boric Acid Solution Using Electrostatic Ion Chromatography
    SHEN Gui-Jun, PENG Zeng-Hui, HUANG Hai-Ying, SHI Yu-Hua, YU Ai-Min, JIN Qin-Han
    1999, 20(10):  1538-1541. 
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    Astationary phase for the electrostatic ion chromatography(EIC) was improved by coating the reversed-phase ODS column with conjugated bile acid salt micelles(CHAPSO). The detector of refactometry was connected on line to the EIC. Using purewater as mobile phase, the separation and speciation conditions of species in boric acid solution were studied. Retention behavior of EICfor ions and molecules in boric acid solutions were discussed.
    UV-Vis Adsorption Spectra Tracing on Photodegradation of Azo Compounds on the Surface of Titanium Dioxide(é) The Discovery and Kinetic Behaviors Researching of Intermadiates
    MA Wan-Hong, CAI Ru-Xiu, LIU Zhi-Hong, LIN Zhi-Xin
    1999, 20(10):  1542-1547. 
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    The kinetics and electron transfer of the photo-degradation procedure of five azo compounds, mainly DBC-carboxyazo, on the surface of titanium dioxide were studied by using UV-V is absorption and differential spectra. An intermediate with rather long life(t1/2=8.86 min) formed and then destructed during the procedure of the capture of the photo-in-duced charge-carrier. The theoretically fit peak-shape curve of the intermediate with error compensated algorithm parallel accorded with the experimental c~t curve. Thus we have got the rate constants of DBC-carboxyazo and TBC-CPA at 25 ℃, being 0.170(k1/min-1) and 2.96×10-2(k2/min-1) as well as 0.104(k1/min-1) and 9.56×10-2(k2/min-1), respectively. The effect of the initial pH value on the photo-degradation rate was tested. pH3-7 was found to be the optimal pH range for the photo-degradation. In addition, the reaction solution without being buffered was found to tend to be weak acidic. The sensitization mechanism of TiO2by azo was discussed. That is, electrons transferred from the excited azo to the conductive band of semiconductor TiO2, which made the bandgap energy match the energy of visible light. The degradation course was presumed as that, after the electron injection and the self-oxidaiton of azo, the intermediate naphthoquinone was oxidized by O2·-to produce phthalic acid, followed by the final mineralization of the phthalic acid to yield CO2, H2O and other inorganic compounds.
    Studies on the Reaction Between Ketorolac, Feprazone and Serum Albumin
    HE Ji-Xiang, JIANG Chong-Qiu, WANG Hong-Jian, WANG Jing-Zheng
    1999, 20(10):  1548-1550. 
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    In this paper, by applying fluorescence quenching method and energy transfer technique, the interaction of serum albumin(BSA and HSA) with ketorolac and feprazone was investigated. The binding sites and binding constants were obtained. According to the thermodynamic parameters, the main sorts of binding force can be known. The results show that two drugs and protein have strong interactions. The mechanism of quenching belongs to static quenching and the main sort of binding force is static-electricity gravitation.
    Determination of the Binding Constant Between Bovine Serum Albumin and Its Monoclonal Antibody by Affinity Capillary Electrophoresis with Laser Induced Fluorescence Detection
    WANG Qing-Gang, LUO Guo-An, William S. B. Yeung
    1999, 20(10):  1551-1553. 
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    The binding constant(Kb) between fluorescein isothiocyanate labeled bovine serum albumin(FITC-BSA) and its monoclonal antibody was determined using the ligand separation mode of affinity capillary electrophoresis(ACE) with laser induced fluorescence detection(LIF). Free FITC-BSA and the complexes were separated by capillary electrophoresis in 7min after incubation. The running buffer was 100 mmol/L HEPE Sat pH7.4, and separation voltage was 30kV. The Kbwas determined to be 4.7×108L/mol using Scatchard plotting method. The influences of incubation time and electrophoresis conditions on determination were also studied.
    Synthesis of N-Benzyl-3(S)-phthalimido-4(S)-[4(S)-2,2-dimethyl-1,3-dioxolan-4-yl]-2-oxo-azetidine
    LI Heng-Guang, WU Tong, XIE Ru-Gang, HU Jian, WANG Jian-Wei, HU Xiao-Bin
    1999, 20(10):  1554-1558. 
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    (S)-Glyceraldehyde acetonide 4 which is a very useful chiraLINtermidiate in stere-oselective synthesis was prepared conveniently by a new three-step synthetic method from natural chiral resource of L-ascorbic acid 1. The chiral aldehyde condensed with benzyl amine to produce adapted chiraLImine 5. The imine is unstable, but it can carry a [2+2] cyclic addition with ketene 8 which was obtained from phthalimidoacetyl chloride and triethylamine under mild conditions, and produce the title compound, N-benzyl-3-(S)-phthalimido-4-(S)-[4(S)-2,2-dimethyl-1,3-dioxolan-4-yl]-2-oxo-azetidine. Because of the high facial stereoselection in cyclic addition mechanism and attacking with ketene in unblocked face of the imine, the optical purity of the final product is quite satisfactory.
    Synthesis and Fungicidal Activity of 3-Anilinomethylene-5,6-dihydro-6-alkyl(aryl)-2H-pyran-2,4-diones
    WANG You-Ming, LI Zheng-Ming, LI Jia-Feng, LI Shu-Zheng, ZHANG Su-Hua
    1999, 20(10):  1559-1563. 
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    3-Anilinomethylene-6-alkyl(aryl)-5,6-dihydro-2H-pyran-2,4-diones(3) were pre-pared by the condensation reaction of 6-alkyl(aryl)-5,6-dihydro-2H-pyran-2,4-diones(1), substituted anilines(2) and ethyl orthoformate. Apair of conformationaLIsomers 4 and 5 exist in products 3 due to the formation of the intramolecular hydrogen bond. Compound 3 was tested in vitro against many fungi such as P. Zeae, C. Arachidicala, P. Piricola, A. Solani, B. Cinerae, S. Sclerotiorum, H. Oryzae, etc . The bioassay results show that they have some fungicidal activity.
    Studies on Semisynthesis and Antibacterial Activity of 3-Heterocyclicthiomethyl Cephalosporins
    HAO Lan, HUI Xin-Ping, ZHANG Zi-Yi, GUAN Zuo-Wu, HE Yu-Lin, YU Hong-Juan
    1999, 20(10):  1564-1569. 
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    Fourteen new mother nucleus of 7-amino-3-heterocyclicthiomethyl cephalosporins 2a_2n were synthesized by the reaction of 7-ACA with 2-substituted 1,3,4-oxadiazol-5-thione-1a_1g, 2-arylamino-1,3,4-thiadiazol-5-thione 1h_1l or 1, 2, 4-triazoline-5-hione 1m, 1n. Two new compounds, 7-(1-aryl-5-methyl-1H-1,2,3-triazol-4-formylamido)-3-(2-substituted-1,3,4-oxadiazol-5-thiomethyl) cephalosporins 4c, 4d, were obtained by the acylation of 7-amino group of 2c, 2d with 1-aryl-5-methyl-1H-1,2,3-triazol-4-formyl chloride 3a, 3b. The structures of the compounds synthesized were confirmed by elementary analyses, IR, 1HNMR and FAB-MS. In preliminary antibacterial sensitivity test, the compounds 2a_2l were found to show higher antibacterial activity than 7-ACA against Gram-positive bacteria, 4c, 4d were found to have significant antibacterial activity against both Gram-positive and Gram-negative bacteria.
    Studies on Synthesis and Complexation Properties of Calix[4] Monothia Crown-5 and Calix[4]monoselenacrown-5
    CHEN Yuan-Yin, CHEN Yi-Kun, LU Xue-Ran, GONG Shu-Ling
    1999, 20(10):  1570-1573. 
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    The synthesis of calix[4]monothiocrown-5 and calix[4]monoselenocrown-5 with sulfur and selenium incorporating into poly(oxyethylene) chains was described. Their structures were confirmed by 1HNMR, MS and elemental analysis. It was shown that the calix-heterocrowns exhibited a high selectivity for Ag+, Hg2+compared with Na+, K+, NH4+, Co2+and Ni2+.
    Synthesis and Bioactivities of Novel 1,3,2-Dioxaphosphorinane 2-one Containing Arylglyoxylonitrile Oxime
    MA Zhi-Hua, SHAO Rui-Lian, MA Hong-Min, CHENG Jun-Ran, HUANG Run-Qiu
    1999, 20(10):  1574-1577. 
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    The reaction of trans-2-chloro-2-oxo-4-phenyl-5,5-dimethyl-1,3,2-dioxapho-sphorinane(Ⅱ) with arylglyoxylonitrile oximes in the presence of PTC resulted in diastereomers of novel cyclic phosphate of arylglyoxylonitrile oxime(Ⅲ). The configuration and ratio of cis/trans diastereomers of Ⅲ were confined by 1HNMR, 31PNMR and X-ray diffraction analysis. The reaction of arylaldoxime with trans-Ⅱ yielded an unstable arylaldoxime cyclic phosphate which was decomposed through Beckmann fragmentation to give nitrile and cyclic phosphate acid. The bioassay indicated that compound cis-Ⅲd showed a high antiviral activity against TMV.
    Studies of Lipases-catalyzed Oleyl Linolenate Synthesis in Nonaqueous Media
    SONG Xin, QU Yin-Bo, HU Xiao-Yan
    1999, 20(10):  1578-1580. 
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    The effects of several lipases on oleyl linolenate synthesis were investigated. The lipase having the highest esterification activity was screened by our laboratory and the yeast which produced this kind of lipase was Trichosporon , named as Y-11. Several factors which influenced oleyl linolenate synthesis were studied. The optimum temperature for the esterification was 30 ℃ and the reaction could be carried out in the temperature range of 4_100 ℃, the optimum pH was 8.0, the optimum substrate concentration was 0.5 mol/L. The esterification rate could amount to 85% after 22h and could further reach 95.2% if the water produced in the reaction was removed in time. Among 11kinds of organic solvents compared, the esterification rate in n-hexane was the highest and that in dimethylsulfoxide was the low-est, the former was ten times higher than the latter.
    Synthesis of 1-Aryloxyacetyl-4-(2-nitrobenzoyl)-thiosemicarbazides and Related Heterocyclic Compounds
    WANG Xi-Cun, YU Tian-Zhi, LI Zheng, CHEN Ji-Chou, WANG Xiu-Chun 
    1999, 20(10):  1581-1583. 
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    Ten new 1-aryloxyacetyl-4-(2-nitrobenzoyl)-thiosemicarbazides(Ⅲ) were synthesized under the condition of solid-liquid phase transfer catalysis, and compounds Ⅲ on fur-ther reaction with acetic acid gives ten 2-(2-nitrobenzoylamido)-5-aryloxymethyl-1,3,4-thia-diazoles(Ⅳ). Compounds Ⅲ and Ⅳ were characterized by elemental analysis, IR and 1HNMR. The preliminary promoting effects of compounds Ⅲ and Ⅳ on wheat growth were also tested.
    Synthesis and Electrochemical Properties of Nanophase MnO2by Solid-phase Reaction(Ⅱ)--Electrochemical Properties of Nanophase γ-MnO2
    XIA Xi, LI Juan, LI Qing-Wen
    1999, 20(10):  1584-1588. 
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    The electrochemical behavior of nanophase γ-MnO2produced by the decomposition of coordination compound precursors and then acid treatment was investigated by using cyclic voltammetry and constant current charge/discharge tests. The results indicated that the nanophase γ-MnO2has a better electrochemical activity than International Common Sample 1(electrolytic mangnese dioxide, abbreviated in S). Their discharge capacities were higher than that of Sespecially at the second discharge step. This favorable performance was more remarkable under the condition of heavy load discharge. Arelatively strong polarization was shown at the beginning of the discharge stage and then strong depolarizable ability in the following stage. CV curves show that the peak current of nanophase MnO2is obviously larger than that of S, and it can be concluded that insertion and deinsertion for protons into the tunnels of crystal lattice of nanophase mangnese dioxide are easier than Safter-0.2 V, and dissolution and deposition for Mn(Ⅲ) and Mn(Ⅱ) species are also easier in nanophase MnO2than in Sin the second discharge step.
    NMR Characterization and Catalytic Hydroform ylation of Water-Soluble Rhodium-Phosphine Com plex in the Presence of Acid and Base
    ZHANG Yu, YUAN You-Zhu, LIAO Xin-Li, YE Jian-Liang, YAO Chun-Xiang, TSAI Khirui
    1999, 20(10):  1589-1594. 
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    When NaOH was added into D2O-solution of HRh(CO)(TPPTS)3[TPPTS: P(m-C6H4SO3Na)3, trisodium salt of tri-(m-sulfophenyl)-phosphine], there were no changes in the characteristic peaks for the w ater-soluble com plex although a sm allpeak at δ35.1 for OTPPTS[OTPPTS: O=P(m-C6H4SO3Na)3, trisodium salt of tri-(m-sulfophenyl)-phos-phine oxide] was formed undera high concentration of NaOH, as evidenced by the spectra of 31P(1H)NMR and 1HNMR, indicating thatthe influence on the m olecular structure ofthe com plex by NaOH may be limited. Severalnew signals at δ29_ 34 accom panied by the ap-pearance of free ligand TPPTSat δ-5.0_-5.3 appeared in the 31P(1H)NMR spectra w hen pyridine w as introduced into HRh(CO)(TPPTS)3, probably due to the reaction of lig-and exchange am ong the coordinated ligands(such as TPPTS, hydrogen, and CO) in the com plex HRh (CO)(TPPTS)3and pyridine m olecule. The w ater-soluble com plex can be readily decom posed, how ever, w hen inorganic acids such as HCl, H2SO4, HNO3and H3PO4w ere introduced into the D2O-solution of HRh(CO)(TPPTS)3, as show n in 31P(1H)NMR spectroscopic data. The decom position of the com plex was com pleted by the form ation of OTPPTS atδ35.1 and som e new phosphate species atδ27_ 29 in the 31P(1H)NMR spectra in the presence ofabove inorganic acids. Analogous results to those by addition ofinorganic acid w ere obtained w hen acetate acid w as exceeded in m ole ratio to HRh(CO)(TPPTS)3An increm entin n/iratio ofheptylaldehydes and a depression in TOF were obtained in case of the addition ofbase, in contrary, a low er n/iratio ofaldehydesin yellow ish productw as ob-tained in case of the addition of acid in 1-hexene hydroform ylation catalyzed by HRh(CO)(TPPTS)3.The results obtained show ed thatthe m olecularstructure and catalytic perform ance of HRh·(CO)(TPPTS)3may be affected by acid more disserviceably than by base.
    Preparation and Characterization of VPO Ultrafine Particles
    ZENG Ling, JI Wei-Jie, CHEN Yi
    1999, 20(10):  1595-1600. 
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    VPO ultrafine particles were first successfully prepared by the supercritical fluid drying(SCFD). BET, XRD, TEM and XPS techniques were used to investigate the specific surface area, the phase composition, the grain size and the oxidation state of various samples. The VPO ultrafine particles after SCFD were activated in the reactant mixture or nitrogen at 673K for 6h. The results indicated that the obtained VPO ultrafine particles have a larger specific surface area, much smaller particle size and an unidentified crystalline phase in some cases after SCFD and activation. The kind and amount of promoter used and the activation atmosphere affect the physical properties of the VPO ultrafine particles. An ultrafine particle with Zr4+and Mo6+promoters, a surface area of 175.6 m2/g and grain size of smaller 50 nm, can be obtained by activating in the nitrogen atmosphere at 673 Kfor 6 h. The oxidation state of surface vanadium atoms of ultrafine particles was around +4, similar to that of vanadium in (VO)2P2O7.The surface P/V molar ratio is in the range of 1.04-1.46, and is a little higher among the samples activated in N2atmosphere. Primary property evaluating results indicated that the small VPOparticles showed very high selectivity but relatively low conversion.
    Effects of Additives on Rheological Properties of TiO2/Water Dispersions
    YANG Hua-Gui, HAN Jin-Yi, GU Hong-Chen, GAN Lu-Ping
    1999, 20(10):  1601-1604. 
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    The effects of additives [N(CH2CH2OH)3,(NaPO3)n(n=10~20), (NH4)2CO3] on rheological properties of TiO2/water dispersions were studied through measurements of shear viscosity, yield stress and thixotropic loops. The results show that TiO2water dispersions exhibit the best disperse property, low viscosity without yield stress when the mass fraction of N(CH2CH2OH)3 is 0.1%; but (NaPO3)n(n=10~20) beheves the time dependence as dispersant for TiO2water dispersions, as flocculation agent in TiO2industry, the concentration of (NH4)2CO3has effects on the rheological properties of TiO2water dispersions.
    Analysis of the Compositions on PET Surface Layer Modified by Fluorocarbon Plasmas with Angle-dependent XPS Technique
    ZHANG Liang, MAO Kun-Yuan, ZHANG Xin-Sheng, WANG Jian-Qi
    1999, 20(10):  1605-1608. 
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    The surface of PET was modified by fluorocarbon plasmas.Angle-dependent XPS technique was employed to study the surface structure and compositions of the modified layer on PET surface. It was found that the homogeneous, cross-linking modified layer on PET surface can be formed by CH4/CF4plasmas, and their composition change a bit with the increase of the sampling depth of XPS. However, for pure CF4plasma, the modified layer is heterogeneous, and the amount of the fluorine-containing groups on the outmost modified layers is more than that in the inner layer. The structures of the modified layer on the modified PETsurface depend on the molar amount of CH4The relationship between the compositions of the modified layers and the sampling depth will be discussed in details in this paper.
    Theoretical Studies of Structures, Electronic Spectra and Nonlinear Second-order Optical Properties of Dicyano[60]fullerene Derivatives
    REN Ai-Min, FENG Ji-Kang, LIU Wen-Ge, SUN Xiu-Yun, FU Wei, JIN Hong-Wei
    1999, 20(10):  1609-1614. 
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    The electronic structures of ground state and electronic spectra of C60C(C≡N)2and C60(C≡N)2were calculated with INDO/2 and INDO/SCI methods. The obtained results are consistent with that of experiment in general. The nonlinear second-order optical susceptibilities βijkand βμ calculations have been performed with ZINDO-SOS method on the basis of correct electronic spectra. Analysis and discussion for the obtained results have been made. The conclusion is that the both molecules C60(C≡N)2and C60C(C≡N)2have a big β value, but C60C(C≡N)2might be expected to be one kind of nonlinear optical materials.
    Studies on Synthesis of para-Isopropylphenol over the P-HZSM-5 Catalyst
    ZHU Rui-Zhi, GUO Chang-Wen, TANG Xiang-Hai, PAN Lü-Rang
    1999, 20(10):  1615-1618. 
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    Alkylation of phenol with isopropanol to para-isopropylphenol(p-IPP) over P-HZSM-5 catalyst has been studied. The influence of phosphorus modification on catalytic performance of HZSM-5 has been investigated. The acidic site density and acid types were determined by means of NH3-TPD and Pyr-IR. The selectivity of p-IPP increased to 95% while the conversion of phenol and the acidic site density decreased on the HZSM-5 after modified with NH4H2PO4.In the preparation of P-HZSM-5, it appeared that there was an interaction between phosphorus and HZSM-5 zeolite, which resulted in framework dealumination on HZSM-5, and calcination influenced both activity and p-IPP selectivity. The selectivity of P-HZSM-5 reached the highest when the support and the catalyst were calcined at 973 Kand 823 K, respectively.
    Reaction Products of 532nm Laser Ablation of Ta with Carbon Dioxide Studied by Matrix Isolation Infrared Spectroscopy
    CHEN Mo-Hua, WANG Xue-Feng, ZHANG Lu-Ning, QIN Qi-Zong
    1999, 20(10):  1619-1621. 
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    532nm pulsed laser-ablated Ta atoms react with carbon dioxide to form products TaCO, OTaCO and O2Ta(CO)2, which have been isolated in argon matrices and identified by their FTIR spectra and a comparison of the spectra of OxW(CO)y. Annealing of matrix isolated sample results in the growth of OTaCO and O2Ta(CO)2, and further 266nm laser irradiation leads to the increase of OTaCO as well as the formation of O2TaCO.
    Gold Nanowires Prepared by Template Synthesis Method
    PAN Shan-Lin, ZHANG Hao-Li, PENG Yong, WANG Zhen, LI Hu-Lin
    1999, 20(10):  1622-1624. 
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    We prepared highly ordered porous aluminum anoxicoxide (AAO)templates containing uniform nanoscale pores. Gold nanowires with lengths up to 2~3 μm and diameter as short as 15 nm were fabricated by ac electrodeposition of gold into the uniform templates. The templates and nanowires were characterized by Transmission Electron Microscope (TEM), the diameter of the resulted nanowires was determined by the pore size of the AAOtemplates, and their length was in proportional to the deposition time. It was also found that the nanowires were composed of many small single crystals and could be as thin as the diameter of one single crystaLIf the pore size of the template was small enough.
    Studies of Surface Photovoltage Spectroscopy on the TiO2Single Crystal(001) Surface
    HUI Zheng, XU Jin-Jie, XIE Teng-Feng, WANG De-Jun, LI Tie-Jin, SUN Jia-Chong
    1999, 20(10):  1625-1627. 
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    We used polarized surface photovoltage spectroscopy (PSPS) to study the photo-voltage response of TiO2single crystal (001) surface. Besides a band-band transition at 355 nm and a indirect transition at 410 nm, we observed a new photovoltaic response at 380 nm in the PSPS spectrum which was assigned to the transition with relation to the surface state. Under different polarized directions, the intensity of photovoltaic responses at 380 nm and 410 nm changed regularly, which proved that the two transitions were interrelated to the atomic arrangement on the TiO2single crystal (001) surface.
    The Intrinsic Viscosity of Polyamidoamine Dendrimer
    LONG Fei, FAN Yu, DING Hui-Jun, JIA Xin-Ru, LI Ming-Qian
    1999, 20(10):  1628-1632. 
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    The intrinsic viscosities of a group of polyamidoamine PAMAM dendrimer, having ethylenediamine as the core, have been investigated. The intrinsic viscosity of G=0.5~4.5 PAMAM shows a maximum at G=2~3, while the ammonium quanternaries show a minimum there. The hydrodynamic radii of PAMAMcalculated from intrinsic viscosity, increase approximately linearly with dendrimer generation.
    Electronic Structure and Luminescent Property of Phenylenevinylene Dimers with Different Electron-releasing Substituents
    SUN Jing-Zhi, CHEN Yu, WU Fang, MA Yu-Guang, TIAN Wen-Jing, SHEN Jia-Cong
    1999, 20(10):  1633-1636. 
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    A series of phenylenevinylene dimers with different electron-releasing substituents were synthesized by Wittig reaction. Their electronic structures were characterized with cyclic-voltammetry and UV-V is spectra, their energy levels were calculated with a quantum chemical calculation approach (AM1), the relationship between the photoluminescent property and the electronic structure was systematically discussed.
    Synthesis of a Photo crosslinked Electro-optic Polymer and Its Electro-optic Measurement
    ZHANG Da-Ming, SUN Jing-Zhi, Hou-A Lin, TIAN Xiao-Jian, MA Yu-Guang, SHEN Jia-Cong, YI Mao-Bin
    1999, 20(10):  1637-1641. 
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    A novel three-dimensional electro-optic polymer containing photo-crosslinkable group was synthesized. 4-Nitroaniline and cinnamyl were introduced onto the polymer matrix of bis-A-epoxy as the electro-optic chromophore and photosensitive chromophore respectively. Athermal stable polymeric electro-optic film was prepared by spin-coating, followed by the corona poling and photo crosslinking reaction in the late poling phase. An external electro-optic measuring system based on the electro-optic film was fabricated, by which the electric-signals propagating on the coplanar waveguide were measured.
    Polyimide Molecular Chains Alignment in Polarized Pulsed Laser Induced Periodic Surface Structures
    LU Qing-Hua, H.Hiraoka, WANG Zong-Guang
    1999, 20(10):  1642-1645. 
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    Periodic nano-lines in a large area have been formed on polyimide surface using polarized pulsed laser-inducing of the fourth harmonic Nd:YAG laser. The linear direction is parallel to the polarization direction and the periodical width of these lines is 200 nm.The dichroism due to the alignments of functional group in periodic nano-structure has been studied by recording polarized reflected FTIR spectra at 0° polarization parallel to the polymer lines and 90 °polarization lines. We found that C=Ostretching at 1722 cm-1in the irradiated area has a stronger response than in the nonirradiated area when the IR polarization direction is parallel to the lines, while the band at 1231 cm-1assigned to C-C-Cbetween phenylenes and the methylene groups has a stronger response when the polarized IRdirection is perpendicular to the lines. The dichroic spectrum indicates that in the irradiated area polyimide molecular chains are preferentially oriented perpendicular to the nano line direction. The orientation is caused by the directional electric field associated with the polarized laser beam during the melting and cooling process, while the polar carbonyl groups are subjected to the orientation in the electric field direction.
    Embedment and Deliverance of 5-Fluorouracil from Blended Membrane of Silk Fibroin and 5-Fluorouracil
    CHEN Jian-Yong, LIU Guan-Feng, SHEN Zhi-Quan
    1999, 20(10):  1646-1650. 
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    The silk fibroin membrane is an amphoteric ion-exchange membrane composed of both weak acidic and weak basic groups. 5-FluorouraciLIs an anti-cancer drug. The condition of 5-fluorouracil blended into silk fibroin membrane has been investigated, then deliverance of 5-fluorouracil from blended membrane of silk fibroin and 5-fluorouracil was measured in the pH range from 3 to 9. The results of SEM, FTIR, DSC show that 5-fluorouracil could be evenly blended into silk fibroin protein. After coating with silk fibroin, the dissolve rate of 5-fluorouracil fixed on silk fibroin and 5-fluorouracil blended membrane could be descended, and the delivery time of 5-fluorouracil could be prolonged. The delivery time and dissolve rate also depends on pHvalues of soaking solution. It is expected that silk fibroin membrane could be used as the matrix of 5-fluorouracil delivery system.
    Prediction, Control and Optimization for Vinyl Monomer/N-Phenylmaleimide Copolymers Composition
    DU Miao, SHAN Guo-Rong, WENG Zhi-Xue, HUANG Zhi-Ming, PAN Zu-Ren
    1999, 20(10):  1651-1655. 
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    The composition change of vinyl monomer/N-phenylmaleimide (PMI) copolymer with conversion was predicted with stepwise calculation method of Mayo-Lew is equation. The composition of copolymer could be controlled and optimized by properly selecting the comonomer and the feed fraction. Based on the characteristics and technology of vinyl chloride/PMI/acrylonitrile copolymerization, the optimum range of monomer feed fraction was obtained.
    Studies on the Glass Transition Temperature of VC/PMI Copolymer
    DU Miao, WENG Zhi-Xue, SHAN Guo-Rong, HUANG Zhi-Ming, PAN Zu-Ren
    1999, 20(10):  1656-1659. 
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    The effects of monomer ratio, temperature, conversion, and feeding modes on the glass transition temperature of VC/PMI copolymer were investigated on the basis of the structure and the feature of copolymerization process. The relationship between glass transition temperature and conversion was predicted by using sequence model and was nearly in agreementwith the experimental data. Portionwise feeding can improve the heat-resistant properties of the copolymer, but lead to worse particle properties.