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Table of Content

    24 June 2000, Volume 21 Issue 6
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    Articles
    Synthesis and Structure of Bis(2,4-dimethylpentadienyl)gadolinium Chloride
    WANG Jian-Hui, MU Ying, SHI Zhan, ZHANG Suo-Bo, FENG Shou-Hua
    2000, 21(6):  829-831. 
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    Anew complex {〔2,4-(CH3)2C5H5〕2GDcl}2 was obtained by the reaction of [2,4-(CH3)2C5H5]3Gd with GDcl3 in toluene at refluxing temperature. The compound {[2,4-(CH3)2C5H5]2GDcl}2 crystallizes in the monoclinic system, space group P21/ n with a =0.89141(18) nm, b =1.4486(3) nm, c =1.15925(15) nm, β = 92.996(18)°, V =1.4949(4) nm3 , Z =3.
    Mass Transfer of Er(Ⅲ) Between HBTMPTP Dissolved in n-Heptane and HAc-NaAc
    YUE Shan-Tang, MA Gen-Xiang, LI De-Qian, SU Qiang
    2000, 21(6):  832-835. 
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    The rate of extraction of Er(Ⅲ) from aqueous acetate solutions at 0.2 mol/Lionic strength by HBTMPTPin n heptane was studied by using a constant interfacial area cell with laminar flow at (30± 0.5) ℃. The interfacial activity of HBTMPTPwas investigated at n heptane/ 0.2 mol/L(H, Na)Ac (pH= 5.00 ) interface. The rate of Er(Ⅲ) extraction was measured aTdifferent chemical compositions by varying hydrogen ion, HBTMPTP, Cyanex 302 and chlorine ion concentrations. The effect of stirring speed, temperature and special interfacial area on the rate of extraction was also studied. The results showed that, under the conditions of the experiments, the overall rate is diffusion controlled. It was found that the impurities of Cyanex 302 have the effect of synergistic extraction.
    Synthesis Crystal Structure and Properties of Binuclear Manganese Complex[(phen)2Mn2(μ-O)(μ-Ac)2(H2O)2](ClO4)2·4H2O
    LI Jun, ZHANG Feng-Xing, TANG Zong-Xun, SHI Qi-Zhen, ZHOU Zhong-Yuan
    2000, 21(6):  836-839. 
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    Binuclear manganese complex [(phen)2Mn2(μ-O)(μ-Ac)2 (H2O)2](ClO4)2·4H2Owas synthesized by the reaction of MnAc 3·2H2Owith phen in the HAc NaAc buffer(pH=4.0). X-ray diffraction result for the single crystal shows that the crystal belongs to monoclinic system, space group P21/n , with a =1.02528(5) nm, b =1.79275(9) nm, c =1.98414(10) nm, β =94.8430(10)°, V =3.6340(3) nm3, Z =4. There is a obsorption peak at 480 nm in UV-Vis spectrum. Cyclic voltammogram shows that the complex in MeOHundergoes a quasi-reversible one-electron redox reaction at E1/2 =0.7 V.
    Synthesis of β-Cyclodextrin and Glucoside Compounds-bonded Porphyrins and Metal Porphyrins
    LI Zao-Ying, LI Cong, LI Li, WANG Tie-Feng
    2000, 21(6):  840-843. 
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    The reaction of mono-6-hydroxy permethylated β-cyclodextrin(PM β-CD-CH2OH) with trifluoromethanesulforic anhydride under N2 gave mono 6 trifluoromethanesulfonate permethylated β-cyclodextrin(6). Compound 6 reacted with 5-( p aminophenyl)-10,15,20-triphenyl nickel porphyrin [NiTPNH2 P](2) or 5-( p aminophenyl)10,15,20 triphenyl carbonyl ruthenium porphyrin[Ru(CO)TPNH2 P](3) to produce complexes 7 and 8. 1-Bromo-2,3,5-Oacetyl-β-D-furanoside(4) and 1-bromo-1,2,3,4,6-Oacetyl-α-D-pyranoglucoside(5) respectively reacted with H2TPNH2 P(1) to afford compounds 9 and 10. The new compounds 6—10 were identified by IR, UV-Vis, 1H NMR, elemental analysis, in which compound 6 was determined by MSspectra.
    Magneto-chiral Effect of Optically Active Metalloporphyrin
    YING Xiao, LIU Hai-Yang, HU Xi-Ming, YAO Zhong-Ping, HUANG Jin-Wang, TIAN Xuan, JI Liang-Nian
    2000, 21(6):  844-846. 
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    Strong magneto chiral effects in absorption of phenylalanine bridged chiral zinc bis porphyrin O,O-C2-Phe-C2 (TPP)2Zn2 were demonstrated through the comparison of natural circular dichroism and magnetic circular dichroism spectra of enantiomers. Magneto-chiral circular dichroism spectra expressed as difference between the absorption coefficients of the left circularly polarized and right circularly polarized light are given. The observed intensive magneto chiral effect was suggested to be related with the chiral exciton coupling between two zinc porphyrin chromophores of the enantiomers.
    Synthesis of the Needle-like Silica Nanoparticles by Biomineral Method
    GUO Zhong-Man, WANG Li-Jun, CHEN Xia, WANG Ce, LI Tie-Jin 
    2000, 21(6):  847-848. 
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    Two aleos was cultured with cultivation solution containing TEOSand no TEOS, respectively. Many needle-like silica nanoparticles was observed by scanning electron microscope in the leaf of aleo cultured with cultivation solution containing TEOS. The results indicated that silica nanoparticles with a special form can be synthesized by biomineral method with leaf cell wall of aleo as templates.
    Studies on Phase Transition of Orthorhombic AlPO4-5 Molecular Sieve by Infrared Spectra
    WEI Bo, YU Ji-Hong, DING Hong, SHAO Chang-Lu, LI Xiao-Tian, QIU Shi-Lun 
    2000, 21(6):  849-851. 
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    AlPO4 5 molecular sieve with an orthorhombic phase was studied by in-situ variable temperature infrared spectroscopy. The reversible phase transition from the orthorhombic into the hexagonal phase was found at about 120 ℃.
    Synthesis of Meso-porous Silica Using Mixed Cationic-nonionic Surfactants as Templates
    BU Lin-Tao, SHAO Qing, DAI Le-Rong
    2000, 21(6):  852-854. 
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    Using the mixture of cationic surfactant cetyltrimethylammonium bromide(CTAB) and six nonionic surfactants as templates, meso porous silica was synthesized. The d space of silica templated by CTABis 3.5 nm. The d spaces could be controlled by changing the ratio of nonionic to cationic surfactants and by increasing the length of nonpolar chain of nonionic surfactants in the mixed cationic-nonionic surfactant templating systems. The pore dimension of silica in the mixed surfactants templating system is larger than that in CTABsystem and a well ordered structure of pore array was maintained.
    A Novel Algorithm Based on the Wavelet Neural Network for Processing Chemical Signals
    CAI Wen-Sheng, YU Fang, SHAO Xue-Guang, PAN Zhong-Xiao
    2000, 21(6):  855-859. 
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    Awavelet neural network based on wavelet analysis can be used to represent chemical signals. The adaptive wavelet neural network using the continuous wavelet transform has problems of a high redundancy and slow training, and the compactly supported orthogonal wavelet neural network using the discrete wavelet transform is difficult to be applied, because the compactly supported orthogonal wavelet function with analytic form is hard to build. Based on the idea of the compactly supported orthogonal wavelet network, a novel algorithm using the compactly supported B-spline function instead of the compactly supported or thogonal wavelet function is proposed. It has been applied to the compression and de- noising of chemical signals. Compared with the adaptive wavelet neural network, the speed of our algorithm was enhanced greatly.
    Studies on Plant Extracellular Calmodulin by Lanthanide Luminescence Probe
    LIU De-Long, SUN Da-Ye, YANG Yan-Sheng, ZHANG Hong-Jie, WANG Shu-Bin, GONG Meng-Lian
    2000, 21(6):  860-864. 
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    Plant extracellular calmodulin(CaM) has been purified from cauliflower and identified with NADkinase(NADK) activation and inhibition effect of CaMantagonist W7. Tb3+ fluorescence titration showed that extracellular CaMcontained four metal-binding sites. The excitation spectrum and emission specturm indicated that extracellular CaMcontained one tyrosine residue which could transfer energy to bound Tb3+ . Based on Förster type nonradiative energy transfer theory, the distances of Tyr→sites Ⅲ, Ⅳ have been determined, these are 1.104 nm(Tyr→Ⅲ, site) and 1.056 nm(Tyr→Ⅳ, site). By studing the effect of CaMantagonist W7 and CaMantibody on Tb3+ sensitized fluorescence, it was found that the binding sites of W7 and antibody were located on the c terminal part of plant extracellular CaMwhich contains domain Ⅲ and domain Ⅳ.
    Fabrication of Chemically-modified Electrode Containing2∶18 Tungstophosphate Anions Based on Sol-gel Technique and Its Electrocatalysis
    LI Li-Dong, LI Wen-Jiang, SUN Chang-Qing 
    2000, 21(6):  865-869. 
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    The anions of Dawson-type tungstophosphate acid were modified on the surface of a carbon paste electrode by the sol-gel technique. The electrochemical behavior of the modified electrode was studied in detail, including pHdependence, stability and so on. Experimental results show that the modified electrode not only maintains the electrochemical activity and electrocatalytic properties of P2W18, but also has a good stability and sensibility. In 0.5 mol/L H2SO4 solution, the third and the fourth cathodic peaks of P2W18 doped in sol-gel film have a good catalytic effect on the reduction of nitrite. The catalytic current is proportional to NO2-concentration. At the same time, we found that the third and the fourth cathodic peaks of P2W18 doped in sol-gel film had an excellent effect on the reduction of dioxygen.
    Determination of Estrodiol by Capillary Electrophoretic Immunoassay with Thermally Reversible Hydrogel
    SU Ping, WANG Yong-Cheng, ZHANG Xin-Xiang, SUN Ling, CHANG Wen-Bao
    2000, 21(6):  870-872. 
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    In this paper, a kind of thermally linear polymer, poly-N-isopropylacrylamide(PNIPA) was packed into capillary electrophoresis, which can be used to separate bound and free estradiol antigen. Auseful method for determination of estradiol in serum by hydrogel capillary electrophoretic immunoassay(CEIA) was developed. The influence of concentration and pHof buffer, concentration of hydrogel, applied voltage, temperature etc has been studied. The limit of detection and the linear range of estrodiol were 30 pg/mLand 0.1—10 ng/mL.
    An Electrochemiluminescence Immunosensor for Determination of Methsulfuron-methyl
    XING Wan-Li, CHAO Fu-Huan, JIANG Zhong-Hua, MA Li-Ren
    2000, 21(6):  873-875. 
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    An electrochemiluminescence(ECL) biosensor based on solid-phase antigen competitive immunoreactions was constructed to determine methsulfuron-methyl using Ru(bpy)32+ as labeling reagent. The coating hapten was bound to the surface of microparticles through avitin-biotin reaction. An electrochemical flow cell containing working electrodes and counter electrodes for initiation of the ECLreaction was constructed. Results showed that the detection limit for methsulfuron-methyl was 0.1 ng/mL.
    The Determination of Isomers of Dihydroxybenzenes by High Performance Liquid Chromatography with ChemiluminescenTdetection
    CUI Hua, HE Cai-Xia, ZHAO Gui-Wen
    2000, 21(6):  876-878. 
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    Based on the inhibition by hydroquinone, catechol and resorcinol of chemiluminescence from luminol potassium hexacyanoferrate(Ⅲ) system, a high performance liquid chromatographic procedure with chemiluminescenTdetection was developed for simultaneous determination of hydroquinone, catechol and resorcinol. The separation was carried out on RP-C18 column at 37 ℃ by using a step gradient elution made by the mobile phases of methanol(A) and 0.05% H3PO4(B). The gradient elution condition was 95% B, 5 min; 95%B-50%B, 1 min; 50% B, 6 min. This method has the merits of high senstivity and good selectivity. The detection limits for hydroquinone, catechol and resorcinol are 2.0×10-9 , 3.2×10-9 and 6.8×10-7 g/mL, respectively. The relative standard deviation( n =5) is 1.9% for 2.5×10-7 g/mLhydroquinone, 1.0% for 7.5×10-7 g/mLcatechol, 4.0% for 5.0×10-5 g/mLresorcinol, respectively. The recovery is in the range of 94%—104%.
    The Synthesis and Thermal Stability of Thioether Dianhydride Poly(amic acid)
    WANG Jiang-Hong, SHEN Yu-Quan
    2000, 21(6):  879-883. 
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    Thioether dianhydride, 2,2'-｛4-[(4-nitrophenyl)azo]imino｝bis ethylamine(diamine monomer) were synthesized and characterized. Due to this chromophore molecule(diamine nonomer) have further polymerizable amino groups on one end of the molecule, the corresponding poly(amic acid) formed with thioether dianhydride exhibited a good solubility in common organic solvents. Decomposing temperature of the diamine chromophore in the poly(amic acid) and polyimide backbone are Td=362 ℃ and 491 ℃, respectively. These polymers are currently showing interesting potential in highly sensitive, nonlinear optical materials.
    Synthesis and Antitumor Activities of Spin Labeled Derivatives of Daunorubicin and Doxorubicin
    MA Cheng, WANG Yan-Guang, CHEN Yao-Zu
    2000, 21(6):  884-887. 
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    Five new spin-labeled derivatives of daunorubicin and doxorubicin(5_9) were synthesized and their structures were identified by IR, MSand ESRas well as elementary analysis. All new compounds were evaluated for their antitumor activities against mouse leukemia P388, B16, human stomach carcinoma SGC-7901 and human liver cancer SMMC7721 cells in vitro. The preliminary results showed that compound 9 was as active as the clinically used doxorubicin.
    Studies on Transition-metal Complexes Containing the Scorpionate Ligand(Ⅰ) Synthesis,Characterization and Crystal Structure of Copper(Ⅱ) Complexes with Hydrotris[3-(p-methoxyphenyl( pyrazol-1-yl) )]borate
    DENG Yuan, WANG Ru- Ji, L I Yong, SUN Shu- Qin, DING Ting- Zhen
    2000, 21(6):  888-893. 
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    A scorpionate ligand K[HB{pzAn}3]( pzAn=3-{p-methoxyphenyl}pyrazole) was prepared, which was reacted with one molar equivalent of Cu( O2 CMe)2 · H2 Oin THFat room temperature, yielding [Cu( O2 CMe) (HB{pzAn}3) ](Ⅰ) .But the reaction of K[HB{pzAn}3]with anhydrous Cu Cl2 afforded CuCl(pzAnH) (HB{pzAn}3) (Ⅱ) .The EPR spectra of Ⅰand Ⅱ in benzene solution exhibit a pseudoaxial symmetrical {dx2-y2}1 configuration at copper.Both Ⅰ and Ⅱ are characterized by IR, elementary analysis and CV.The crystal structure of compound Ⅱ has been determined.Crystals are monoclinic,space group P21/c with a=1 .1643( 2 ) nm,b=2 .7081 ( 5) nm,c=1 .4494( 3) nm,β= 10 5.37( 3)°,V=4.4066( 14) n m3 and Z=4,with final residuals R=0 .0604 and Rw=0 .1416.The complex shows a distorted square pyramidal copper center,and exhibits a weak intramolecular hydrogen bond,N_ H… Cl,with bond length of Cl… N 0 .300 9nm and bond angle of Cl… H _ N 12 0 .3°.
    Studies of CO Selective Reduction of Aromatic Nitro Compounds in Water/Organic Phases by Using Ru3(CO)9(TPPTS)3
    MEI Jian-Ting, JIANG Jing-Yang, XIAO Qi-Ming, LI Ya-Ming, JIN Zi-Lin
    2000, 21(6):  894-897. 
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    Ru3(CO)9(TPPTS)3 was used in the selective reduction of aromatic nitro compounds under COatmosphere in water/organic biphase system. It was found that the reaction was accelerated obviously by phase-transfer catalysts and the cetyltrimethylammonium bromide(CTAB) is the best one among them. Using o-ClC6H4NO2 as a reactant, the influences of the concentration of CTAB, the concentration of NaOH, reaction temperature and COpressure on the catalytic properties of Ru3(CO)9(TPPTS)3 were studied. Under the conditions of 120 ℃, pco =4 MPa, 3 mol/L NaOH, 8 h, both the conversions of o-ClC6H4NO2 and the selectivity of o-ClC6H4NH2 were 99.9%. The reductions proceeded with a markable activity and selectivity toward aromatic nitro group as C-O, C-Ngroups present in the substrate. After 3 times recycle of the catalyst the conversion of o-ClC6H4NO2 and the yield of o-ClC6H4NH2 were more than 92%.
    Reaction of 1,1'-Bis(tetramethylcyclopentadienyl)ferrocene with Pentacarbonyl Iron and Triacetonitrile Tricarbonyl Molybdenum
    DENG Xiao-Bin, XU Shan-Sheng, WANG Bai-Quan, ZHOU Xiu-Zhong 
    2000, 21(6):  898-902. 
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    The xylene solution of 1,2-bis(tetramethylcyclopentadienyl)ferrocene, 1,1'-Fc(Me4Cp)2(Ⅰ) and Fe(CO)5 was refluxed for 10 h to yield ferrocene bridged bis(tetramethylcyclopentadienyl) tetracarbonyl, 1,1'-Fc[(Me4Cp)Fe(CO)2]2(1). Futher reaction of compound 1 with I2 in chloroform to yield Fe_Fe bond cleaved product, 1,1'-Fc[(Me4Cp)Fe(CO)2I]2(2). compound Ⅰ reacted sequentially with n BuLi and Mo(MeCN)3(CO)3 to generate 1,1'-Fcbis[tetramethylcyclopentadienyltricarbonyl molybdenum anion salt], 1,1'-Fc(Me4Cp)Mo(CO)3-Li+]2(Ⅱ). Futher reaction of compound Ⅱ with MeIyielded the corresponding methylmolybdenum complex, 1,1'-Fc[(Me4Cp)Mo(CO)3Me]2(3). The reaction of compound Ⅱ with BrCH2CH2Br did not gave the expected Mo_Mo binuclear compound, instead a small quantity of ferrocene bridged bis(molybdenum bromide) compound, 1,1'-Fc[(Me4CpMo-(CO)3Br]2(4), which was isolated by nucleophilic substitution and elimination mechanism. The molecular structures of compounds 1_4 were characterized by elemental analyses, IRand 1H NMRspectra. The crystal structure of compound 1 was determined by X-ray diffraction.
    Synthesis and Characteristics of Compounds Having Both Photochromic and Fluorescent Character
    PANG Mei-Li, WANG Yong-Mei, MENG Ji-Ben, WANG Ji-Tao
    2000, 21(6):  903-907. 
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    Eight new compounds which have both photochromic and fluorescent character have been synthesized by esterification reaction in the presence of DCC from the derivatives of indolinospirobenzopyrans and coumarins. The structure of these new compounds were identified and their spectrum properties were studied. The new compounds were shown to be have both photochromism character and fluorecent character, and their fluorescent spectrum have two exciting wavelength and two different emitting peak respectively. They were expected to be applied in such areas as anti forgery materials, bio-labeling reagents, and other multiple functional materials.
    Ab Initio Studies on the Hydride of “Met-Cars” Ti8C12H4 and Ti8C12H8
    CUI Meng, FENG Ji-Kang, WANG Su-Fan, GE Mao-Fa, SUN Jia-Chung
    2000, 21(6):  908-911. 
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    The geometrical structures of Ti8C12 with Td symmetry is optimized by quantum chemical ab intitio method. The result shows that the property of Ti8C12 in chemical reaction is reactive. The geometrical structures with Td symmetry of hydride of Ti8C12 is also explored by the same method, the stablity and reactivity of Ti8C12 H4(Td) and Ti8C12 H8(Td) is predicted. As a result, Ti8C12 H4(Td) is more stable than Ti8C12 (Td) and Ti8C12 H8(Td), moreover, Ti8C12 (Td) and Ti8C12 H8(Td) have similar stability. Thus, it can be indicated that Ti8C12 H4(Td) and Ti8C12 H8(Td) cluster can exist.
    Theoretical Study on the Mechanism of Electrochemical Reduction Reactions of Honokiol
    SUN Cheng-Ke, GONG Si-Yuan, LI Zong-He, MA Si-Yu, LI Qi-Long
    2000, 21(6):  912-917. 
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    The mechanism of electrochemical reduction reaction of 2-(3-allyl-4-hydroxyl)-phenyl-4-allyl-phenol, also named honokiol, has been studied by using the sem i-empirical molecular orbital AM1 and PM3 methods. The results show that these reduced positions of honokiol molecule are two double bonds of o allyl and p allyl groups, and the o-allyl group is reduced first, then the p-allyl group. The honokiol gets 4e and 4H+, and the two allyl groups are saturated in the reduction process. The calculated results are in good agreement with experimental facts.
    Electronic Structures and Stabilities of Hypervalent Lithium-sodium Combined Oxides OLinNa2(n=1-4) and OLi2Na Species
    ZHENG Xiang-E, WANG Zhi-Zhong, TANG Au-Chin
    2000, 21(6):  918-921. 
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    All possible geometries of hypervalent lithium-sodium combined oxides OLin Na2( n =1—4) and OLi2Na species were determined by B3LYP-DFTmethod with 6-31G* basis set, and the frequency calculations were done on their optimized geometries. The global minima of OLi2Na and OLin Na2( n =1—3) species were all calculated to be C2v structures, and the OLi4Na2 species adopts D2d configuration as its most stable geometry. The global minima of them were calculated to be thermodynamically stable. To dissociate one Li atom, the energies of 212.25432, 68.49208 and 245.55896 kJ/mol are needed for OLin Na2( n =2, 3, 4) molecules, respectively.
    Monte Carlo Simulation to the Effect of Cluster Brownian Diffusion Coefficient on the Colloidal Fractal Cluster Aggregation Kinetics
    WANG Hui, WANG Gui-Chang, CAI Zun-Sheng, PAN Yin-Ming, ZHAO Xue-Zhuang
    2000, 21(6):  922-925. 
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    The aggregation rate constant embodies the microscopic details of the collision process among clusters and the kinetic behavior directly depend on the size and configuration of the reacting clusters. Using Monte Carlo method for different geometric morphologies the diffusion limited aggregation mechanism in three dimensions was randomly simulated. The effect of cluster Brownian diffusion coefficient on the aggregation rate constant for dimers formation, the aggregation rate of the system and the mean cluster size was studied on microscopic and mesoscopic levels.
    The Basis Vectors of f3 Ions in Tetragonal Field and Matrix Elements Related
    ZHOU Yu-Bing, SHA Kun-Yuan
    2000, 21(6):  926-929. 
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    By means of the single electron basis vectors matched for group chain [(O⊃D4⊃C4)×SU(2)] , the Slater functions of the direct product for single electron can be used as the basis vectors of the irreducible represents of fN ions. The Coulomb, Casimir, spin-orbit coupling and crystal field interacting matrix elements in tetragonal field have been described.
    Thermodynamic Study on Separation of Molecular Imprinting Chiral Stationary Phase
    WANG Jin-Fang, ZHOU Liang-Mo, LIU Xue-Liang, WANG Qing-Hai, ZHU Dao-Qian
    2000, 21(6):  930-933. 
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    The effect of temperature on the chiral separation of the molecular imprinting polymer was investigated and the thermodynamic parameters were calculated. It was found that the chiral separation process was enthalpy-controlled. Increasing the temperature decreases the capacity factor and chiral selectivity factor. The interactions between the analyte and the molecular imprinting chiral stationary phase were both non-specific and specific, and only the difference of specific interaction results in the chiral separation. The imprinting cavities affected the thermodynamic parameters dramatically. The rebinding of the imprinted molecule into the imprinting cavities was favorable in view of energy and configuration because of their best compatibleness.
    Studies on the Refined X-ray Powder Diffraction Pattern and Indices of Sodium Hydroxyacetate
    WANG Xi-Wen, LU Xiao-Quan, GAO Jin-Zhang, KANG Jing-Wan
    2000, 21(6):  934-936. 
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    No diffraction data of Sodium Hydroxyacetate(sodium glycolate) has been reported in X-ray powder diffraction files. It is shown that the result of index research of the X-ray powder diffraction pattern of sodium hydroxyacetate was refined carefully. The refined unit cell parameters for orthorhombic system of sodium hydroxyacetate are: a =1.0581(1) nm, b =0.6440(1) nm, c =0.5303(1) nm, V =0.3613(1) nm3 , Z =4 , Dx=1.802 g·cm-3 , Dm=1.786 g·cm-3 , F20 =38, F30=51(0.0088, 68), F59=48(0.0081, 153). Extinction conditions indicate that the space group is P21212(18).
    IR Spectra at Various Temperatures for Polyalchohols
    ZHANG Jian-Ling, LIU Xiao-Di, HE Shu-Mei, WU Ke-Zhong-ZHANG Jian-Jun, FENG Hai-Yan
    2000, 21(6):  937-940. 
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    Aset of series of polyalchohols derived from neopentane[C(CH3)4] by means of the substitution of —CH3 by other groups such as —CH2OHand —NH2 exhibit crystalline transformations which reversibly absorb large amounts of heat and can be used in thermal energy storage. The solid-solid phase transitions of pentylglycol(NPG), pentaglycerine(PG), pentarythritol(PE) and tris(hydroxymethyl)aminomethane(TAM) were studied by infrared spectroscopy at various temperatures and differential scanning analysis. Infrared spectra of four polyalchohols at room temperature show a strong absorption centered at 3300 cm-1 which is identified as the —OHstretching band and indicate that between molecules there are hydrogen bonds which play a dominant role to the structure of low temperature phase(ordered phase). In the temperature range closely corresponding to the solid-solid phase transition —OHstretching band shifts to a higher wavenumber, which indicate that the hydrogen bands between molecules are broken. The out of plane deformation of the OHgroup which is rather sensitive to molecular interactions was also analyzed. Its frequency deviation to lower wavenumber with the increase of the temperature also indicate that the hydrogen bands are broken. The enthalpies and temperatures of solid solid phase transitions for polyalchohols measured by DSCmethod are consistent with the results of IRwhich can declare the mechanism of solid solid phase transition of polyalchohols. With the breaking of hydrogen bonds between molecules and the introduction of vibrational and rotational disorder polyalchohols exhibt crystalline transition. The structure of the high temperature phase which are known as orientationally disordered crystals(ODIC) or plastic phase are face centered cubic for NPG, PG, PEand body-centered cubic for TAM, which can be accounted for the difference between CH2OHand NH2 interactions.
    Thermoregulated Phase-transfer Catalysis ——Recent Advances in Water/Organic Biphasic Catalysis
    JIN Zi-Lin, MEI Jian-Ting, JIANG Jing-Yang
    2000, 21(6):  941-946. 
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    Water/organic biphasic catalysis provided a kind effective way for solving the problem of difficulty from recovering the catalyst in homogeneous catalysis theoretically and practically. So far its application range has been seriously restricted by the water solubility of the substrates. Such a restriction will be fundamentally eliminated by thermoregulated phase-transfer catalysis. The principle of the thermoregulated phase-transfer catalysis, the design and synthesis of thermoregulated phase-transfer ligands and their application in the water/organic two phase-hydroformylation of higher olefins severally insoluble in water, were systematically introduced.
    A Method for Increasing the Three-phase Reaction Boundaries in Anode of SOFC
    HUANG Xi-Qiang, LU Zhe, LIU Wei, LIU Zhi-Guo, PEI Li-HE Tian-Min, LIU Jiang, SU Wen-Hui
    2000, 21(6):  947-948. 
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    Anew method for increasing the three-phase boundaries in anode of SOFCis reported. The results of the study show that the three-phase boundaries in the SOFCanode Ni+YSZare greatly increased by doping Ce0.9Ca0.1O2-δ particles , and the transportation of oxygen ion in the anode is improved as well. By adding Ce0.9Ca0.1O2-δ particles, the composite anode is produced and the anode reaction is accelerated, resulting in an improvement of SOFCoutput properties. The highest power density of SOFCwith the anode of Ni+YSZdoped by Ce0.9Ca0.1O2-δ particles in a weight ratio of 15%, which is about 3 times higher than that of SOFCwith the anode Ni+YSZwithouTdoping, is obtained.
    Synthesis of MCM-22 at Low Na Content Under Dynamic Condition and Catalysis for Non-oxidative Aromatization of Methane
    XU Ning, KAN Qiu-Bin, LI Xue-Mei, LIU Qing-Sheng, WU Tong-Hao
    2000, 21(6):  949-951. 
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    Highly pure crystalline MCM-22 was synthesized under the conditions of a high temperature, low content of Na and water in a short time without addition of the crystal seeds of MCM-22. MoO3 supported by H MCM-22 as the catalyst of the reactions of non-oxidative aromatization of methane is investigated and it is evident that MCM-22 is a promising catalyst support for the studied methane aromatization reaction.
    ESR Study of Intermediates in Electroreduction of 3-Hexyne-2,5-diol
    YUAN Guo-Wei, ZHANG Jing-Dong, SONG You-Qun, HUANG Shu-Kun, SUN Jian
    2000, 21(6):  952-954. 
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    The intermediates of electroreduction of 3-hexyne-2,5-diol at platinized platinum electrode in perchlorate aqueous solutions with various pHvalues have been studied by using electrochemical ESRtechnique with the spin trap phenyl tert butyl nitrone. The six-line spectra in the three solutions with 1.5, 3.5 and 5.0 pHvalues could be ascribed to the form of the radicals, such as CH3C·HC——CCH2CH3 , in the process of producing 3-hexyne. The four-line spectra, increasing in their intensities with increase in pHvalues from 1.5 to 5.0, show that a 2-hydroxyalkyl radical CH3C·(OH)CH=CHCH(OH)CH3 is formed via the interaction between the atom Hand intermediates 3-hexene-2,5-diol and/or CH3C(=O)·CH-CHCH(OH)CH3.
    Studies on Preparation of Carbon Aerogels
    GAN Li-Hua, LI Guang-Ming, ZHU Da-Zhang, YUE Tian-Yi, CHEN Long-Wu
    2000, 21(6):  955-957. 
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    Anew method for preparing carbon aerogels by using starch as a starting material through sol gel process, followed by supercritical drying and pyrolysis is described. The resulting aerogels which consist of irregular carbon particles with sizes about 20 nm were of uniform sizes, low density, porous monolithic materials with a bulk density of 108 kg·m-3 and an electrical conductivity of 1.6 S·cm-1 . The regular arranging crystal structure in manometer dimensions was observed by using high-resolution transmission electron microscopy and electron diffraction. The results of DTA-TG studies indicated that when starch aerogels were heated, the carbon aerogels with graphite structure formed through dehydration, pyrolysis and subsequent phase transition.
    The Photocatalytic Properties of Transition Metal Ion doped TiO2 Nanoparticles ——Photocatalytic Degradation of Rhodamine B
    WANG Yan-Qin, ZHANG Li, CHENG Hu-Min, MA Ji-Ming
    2000, 21(6):  958-960. 
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    The transition metal ion-doped TiO2 nanoparticles were prepared with hydrothermal method, and the effects of doping different metal ions on the ability of TiO2 in photocatalyzing degradation of rhodamine B(RB) were studied. The results showed that the doping of Fe 3+ , Co2+ , Ni2+ and Cr3+ in TiO2 nanoparticles made the photocatalytic efficiency of the TiO2 particles reduce and the higher the initial content of Fe3+ , the lower the ability of TiO2 in photocatalyzing the degradation of RB. But the doping of Zn2+ and Cd 2+ , especially Zn2+ , made the photocatalytic efficiency of the TiO2 particles enhance, showing a great increase of the rate constant(k) and the initial reaction rate(rini).
    Chemical Components and Solution Properties of a Glycan-Protein Complex from Ganoderma Lucidum Mycelium
    CHEN Jing-Hua, ZHANG Li-Na, YU Deng-Shou, ZHU Rong-Ping
    2000, 21(6):  961-964. 
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    A glycan-protein complex (GLM-A) was isolated from the Ganoderma lucidum with phosphate buffer solution at 80 ℃. The carbohydrate in GLM-Ais almost constituted by glucose, and the content of protein is about 13%. The molecular weight Mw dependences of intrinsic viscosity [η] and root mean square radius of gyration 〈 S2〉1/2 of GLM Ain the 1∶1 water diluted cadoxen at 30 ℃ are [ η ]=5.1×10-2 Mw0.60 (cm3·g-1 ) and 〈 S2〉1/2=3.9×10-2Mw0.50(nm), respectively. According to Bohdanecky's method based on Yamakawa Fujii Yoshizakis theory for worm like chain cylinder, molar mass per unit contour length M L, persistence length q , and chain diameter d were estimated to be (530±10) nm-1 , (2.8±0.2) nm, and 0.75 nm, respectively, in the 1∶1 water-diluted cadoxen. The results indicated that the glycan protein complex exists as a random coil in the aqueous solution.
    A Study of the Polymerization of 3-Azidomethyl-3-nitratomethyloxetane
    LEI Xiang-Yang, FENG Zheng-Guo, YANG Ya-Ming, LIU Li-Hua
    2000, 21(6):  965-968. 
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    An improvement on the synthesis of 3-azidomethyl-3-nitratomethyloxetane(AMNO) was performed. With boron trifluoride etherate(BF3·Et2O) as an initiator and butane-1,4-diol(BDO) as a co-initiator, the homopolymerization of AMNOwas investigated in detail by a cationic ring opening polymerization process. The prepolymers show predictable molecular weights and low dispersities. The molecular structures of the polymer were characterized with FTIR, 1H NMRand GPC.
    The Mechanism of Thermal Decomposition of DDS and DR in Aqueous Solution Delayed by SDS
    YANG Bo-Xuan, CAO Wei-Xiao 
    2000, 21(6):  969-975. 
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    The thermal decomposition of diphenylamine diazonium salt(DDS) as the model compound and diazoresin(DR) in aqueous solution of sodium dodecyl sulfate (SDS) was investigated. The results show that the increasing of thermal stability of DDSand DRin SDSaqueous solution is ascribed to the participating of them into the premicelle or micelle of SDSvia the hydrophobic interaction as well as electrostatic attraction between DDS(or DR) and SDS. As a result, the diazonium groups of DDS(or DR) are protected by SDSagainst thermal decomposition. It is also confirmed that the thermal stability of DDSor DRis related closely to the concentration of SDSand salt(NaCl) existing in solution and increases with increasing [SDS] and [NaCl]. It is a reality that the more participation of DDS(or DR) into premicelle or micelle, the more thermal stability of DDS(or DR). Thus, the premicelle form at a low concentration of SDS(≈1×10-5 mol/L) and exert the protection of DDR(or DR) towards thermal decomposition.
    Fluorescence Spectra of Pyrene Labeled Polyelectrolytes with Sulfonate Groups in Water and DMSO
    GAO Feng, YAN Yu, REN Bi-Ye, TONG Zhen
    2000, 21(6):  976-979. 
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    Pyrenylmethyl methacrylamide(PyMA) was synthesized, and applied to copolymerizing with AMPSand DMAAto get a series of pyrene labeled polymers with sulfonate groups. The molar fraction of sulfonate monomer AMPSin these samples varies from 0.0326 to 0.896 . In DMSOand water, the profile of fluorescence spectrum of pyrene labeled polyelectrolytes is analogous to that of PyMAwhen FAMPS < 0.449, while the [0,1] emission peak abruptly increased as FAMPS ≥0.449. The so called polarity scale of pyrene, I1/ I3 of pyrene labeled polyelectrolytes in DMSOand in water decreases gradually with increasing FAMPSrepresenting the charge density of the samples. I1/ I3 also decreases gradually with the increase in polymer concentration in water. The results imply that there exists the hydrophobic aggregation through locally electrostatic attraction even in polyelectrolyte/polar solvent system, in contrast to the traditional polyelectrolyte theory. However, I1/ I3 of these polyelectrolytes remains almost a constant with increasing NaCl concentration of aqueous solution up to 0.75 mol/L, indicating the electrostatic attraction cannot be simply screened.
    Synthesis of PSt-b-PBA-b-PSt and PMMA-b-PBA-b-PMMA Triblock Copolymers by Atom Transfer Radical Polymerization with Ethyl α,α-Dibromoacetate as Difunctional Initiator
    FU Zhi-Feng, LIU Hai-Tao, SHI Yan, JIAO Shu-Ke
    2000, 21(6):  980-982. 
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    Ethyl α,α-dibromoacetate was confirmed to be a difunctional initiator for the atom transfer radical polymerization of n-butyl acrylate by means of gel penetration chromatography. When the polymerization of n-butyl acrylate was carried out aTdifferent molar ratios of ethyl α,α-dibromoacetate and ethyl α bromopropionate with CuBr/2,2′-bipyridine as the catalyst, polymers with bimodal molecular weigh Tdistributions were obtained, consisting of two narrowly distributed fractions, one of which was of a molecular weigh Td ouble the other. Poly( n-butyl acrylate) obtained with ethyl α,α-dibromoacetate as the difunctional initiator was further used as the macroinitiator for styrene and methyl methacrylate in the presence of CuBr/2,2′-bipyridine respectively to prepare ABAtriblock copolymers. It was found that high blocking efficiency was obtained for styrene. However, the polymer with bimodal molecular weighTdistribution was obtained for methyl methacrylate with a low molecular weight peak corresponding to that of poly( n-butyl-acrylate) macroinitiator. If the blocking polymerization was conducted with CuCl/ 2,2′-bipyridine as the catalyst to replace CuBr/2,2′-bipyridine, a high blocking efficiency was also obtained.
    Brill Transition of Nylon1012
    LI Yong-Jin, YAN De-Yue, ZHU Xin-Yuan, JIANG Xu-Lin
    2000, 21(6):  983-984. 
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    Variable-temperature X-ray diffraction(XRD) was used to investigate the crystalline transition of Nylon1012 The results show that Nylon1012 undergoes a crystalline relaxation between the glass transition temperature and the melting point. We thus demonstrate, for the first time, the presence of the Brill transition in Nylon1012, a phenomena that has been extensively studied in Nylon 66. It is found that the Brill transition temperature is about 120 ℃ and we have also showed that the Brill transition of Nylon1012 is reversible when cooling the high temperature pseudohexagonal structure to room temperature.
    Design and Synthesis of a Series of Novel Mesogen-Jacketed Liquid Crystal Polymers
    TU Hui-Lin, YU Zhen-Ning, WAN Xin-Hua, CHEN Xiao-Fang, ZHOU Qi-Feng
    2000, 21(6):  985-987. 
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    This paper describes the synthesis and free radical polymerization of 2,5-bis(4′-alkyloxyphenyl)styrene(M-n) for mesogen jacketed liquid crystal polymers(MJLCPs), where p terphenyl subsituted by alkoxy groups at both ends was used as mesogenic unit. Because of the absence of the polar linkage groups, such as —COO— or —CONH— as employed in the previous reported MJLCPs, Mn is believed to be polymerized easily by both free radical polymerization and ionic polymerization. The chemical structure of Mn was proved by 1H NMR, mass spectrometry and elementary analysis. Their phase transition and liquid crystallinity were characterized by DSCand POM. Although M-1, M-2, M-3 and M-4 exhibited monotropic nematic mesophase, M-5 displayed enantiotropic nematic mesophase presumably because of its decreased melting transition temperature. All monomers were easily polymerized to moderately high molecular weight polymers. At elevated temperature above Tg, poly[2,5-bis(4′-alkoxyphenyl)styrene] showed a very stable mesophase. The formed birefrigence did noTdisappear until thermal decomposition started. Compared to other MJLCPs, the polymers reported here have much higher thermal stability.
    The Single Crystal-like Banded Textures in the Films of a Thermotropic Liquid Crystalline Poly(aryl ether ketone) Containing a Lateral Chloro Group
    FU Lu-Xiang, ZHANG Shan-Ju, ZHANG Jian, LIU Jing-Jiang, YANG De-Cai, SUN Hui, WANG Gui-Bin, WU Zhong-Wen 
    2000, 21(6):  988-990. 
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    The banded textures in the films of a thermotropic liquid crystalline poly(aryl ether ketone) containing a lateral chloro group have been studied by means of transmission electron microscopy(TEM), electron diffraction(ED) and atomic force microscopy(AFM). The crystallization induced banded texture without external shear can be formed when the thin films were annealed at the temperature range(320—330 ℃) of the liquid crystalline state from the melt. The results show that the banded regions have high orientation of single crystal based on the orthorhombic packing and the growing direction of the bands is along the b axis of the crystals. This kind of single crystal like bands is due to the different orientation of the packing molecular chains. The molecular chains of the dark bands in the bright field electron micrograph are perpendicular to the film plane, while the ones of the bright bands are tilt along the b axis with the tilt angle upto ±20°.
    Structure Characterization of Polyhydroxyalkanoates Produced from Activated Sludge in Waste Water Treatment Process
    ZHENG Yu-Dong, ZHONG Qin-Hua, MA Wen-Shi, HUANG Jiong-Liang
    2000, 21(6):  991-993. 
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    It is found that a number of microorganisms in activated sludge in the process of waste water treatment can produce a variety of nomo-and co-poly-3-hydroxyalkanoates with a wide range of properties, which would be one of the methods to low the cost of PHA. In this paper, the biosynthesis of polyhydroxyalkanoates(PHA) by mixed bacterium growth on waste water was studied. The chemical structure of PHA, isolated from activated sludge in waste water treatment process using sodium acetate as attachment carbon source, was analyzed by 1H NMRspectroscopy and gas chromatography mass spectrometry. The PHAproduced from activated sludge is a copolymer composed of 9 different monomer units, 3-hydroxybutyrate, 4-hydroxypentanoate, 3-hydroxydodecanoate, 3-hydroxy-tetradecanoate, 3-hydroxy-9-hexadecenoate, 3-hydroxyhexadecanoate, 3-hydroxy-11-octadecenoate, 3-hydroxy-9-octade-cenoate, 3-hydroxyoctadecanoate.
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