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Table of Content

    24 January 2003, Volume 24 Issue 1
    Preface
    The Preparation of (La,Gd)PO4:RE3+ (RE=Eu, Tb) by Co-precipitation Method and Their VUV Spectroscopic Properties
    WU Xue-Yan, YOU Hong-Peng, ZENG Xiao-Qing, HONG Guang-Yan, KIM Chang-Hong, PYUN Chong-Hong, YU Byung-Yong, PARK Cheol-Hee
    2003, 24(1):  1-4. 
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    (La,Gd)PO4:RE3+ (RE=Eu or Tb) phosphors were prepared by co-precipitation method. It was found that the IR spectra of LaPO4 and GdPO4 were quite similar, the difference was that both stretching frequencies and bending frequencies of GdPO4 were higher than those of LaPO4. The VUV excitation intensity of (La,Gd)PO4:RE3+ is enhanced with the increasing of Gd3+ content, implying the intermediate role of Gd3+ in energy transfer from host absorption band to RE3+. It was also found from XPS that the LaPO4 valance band was formed by the 2p level of O2-, whereas the GdPO4 valance band was composed of the 2p level of O2-and the 4f level of Gd3+, showing the differences in band structures between LaPO4 and GdPO4, which may have influence on the VUV spectroscopic properties of (La,Gd)PO4:RE3+.
    Synthesis of Hierarchically Arrayed Silica Nanorods via Reverse Amphiphilic Block Copolymer Mesophases
    YU Cheng-Zhong, TIAN Bo-Zhi, FAN Jie, TU Bo, ZHAO Dong-Yuan
    2003, 24(1):  5-8. 
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    A reverse amphiphilic mesophases approach to create hierarchically arrayed silica nanorods has been demonstrated. In nonpolar solvent systems, the cylinder nanorods with a uniform diameter(10 nm) generated from highly ordered two-dimensional(2D) reverse hexagonal mesophases are aligned within lamellar macrostructures(150 nm). The diameter size of silica nanorods can be adjusted from 9 to 15 nm by varying the chain length of the EO segment and the concentration of the surfactants. Low surfactant concentration and long hydrophilic EO segment chain yield silica nanorods with a large diameter. The calcined material has a relatively small surface area of 275 m2/g. This approach may provide a new pathway to the fabrication of nano-objects that might be applied in nanoscale devices.
    Studies on the Structure and Properties of Unsymmetrical Tetradentated Schiff Base Ni(Ⅱ) Complex
    XU Xian-Xiu, MU Zhong-Cheng, GUO Li-Ping, WANG Mang, LIU Qun, XING Yan, HU Ning-Hai, JIA Heng-Qing
    2003, 24(1):  9-12. 
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    A new unsymmetrical tetradentated Ni(Ⅱ) Schiff base complex of 3-{1-[2-(3-hydroxy-1-methyl-but-2-ebylideneamino)-pheno-ylimino]-ethyl}-4-methylthio-penta-2,4-dien-2-ol (2) was synthesized in one pot via the reaction of nickel(Ⅱ) acetate, o-phenylene diamine, and 5-(2-acetyl-1-methylthio-3-oxo-butylidene)-2,2-dimethyl-dioxane-4,6-dione (1). Compound 2 was characterized by elemental analysis, IR, 1H NMR spectra, X-ray diffraction patterns and cyclic voltammogram method. The crystal of complex 2 belongs to monoclinic space group: P21/C, with a=1.147 6(2) nm, b= 1.178 2(2) nm, c=1.481 0(3) nm, β=111.73(2)°, V=1.860 2(7) nm3, Z=4, Rf=0.053 5.
    Structural and Magnetic Properties of (Nd1-xYx)3Fe27.31Ti1.69 Compounds
    WANG Wen-Quan, ZHANG Xi-Feng, SU Feng, WANG Xiang-Qun, DU Xiao-Bo, JIN Han-Min, YANG Fu-Ming, WU Guang-Heng
    2003, 24(1):  13-16. 
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    The structure and magnetic properties of Nd1-xYx)3Fe27.31Ti1.69(0≤x≤0.6) compounds have been investigated by means of X-ray diffraction and magnetic measurements. It was found that all the compounds investigated crystallize in Nd3(Fe,Ti) 29-type structure with space group A2/m. With increasing Y content x, the lattice constants and the unit-cell volume decrease monotonically and the Curie temperature Tc reduces slightly. The saturation magnetization M s decreases monotonically with increasing x, which is in good agreement with that expected by a simple dilution model. All the compounds show a spin reorientation at low temperatures and the spin reorientation temperature Tsr decreases with increasing x from232 K(for x=0) to 121 K(for x=0 6). Based on investigation of magnetocrystalline anisotropy, a tentative spin phase diagram has been constructed for the (Nd1-xYx) 3Fe 27.31Ti 1.69(0≤x≤0 6) compounds.
    Studies on the Synthesis and Antitumor Activity of Polyoxometalate Based Liposome Nanocomplex
    WANG Xiao-Hong, WANG Li-Min, LIU Jing-Fu
    2003, 24(1):  17-20. 
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    Liposome encapsulated polyoxometalate α-K8H6[Si2W18Ti6O77](α-Si2W18Ti6) was synthesized by using liposomal encapsulating method. The structure of nanomaterial were characterized by IR spectra, solid NMR spectra and polarography, and the forms and range in size of the nanomaterial were estimated by using TEM and Zetasizer. The results show that the polyoxometalate in the complex retains its parent structure, and the sizes of the complexes are from 60 to 150 nm. By using MTT method, the antitumoral activities of the complexes were assayed. The results showed that after being encapsulated by the liposome, the stability and antitumoral activity of polyoxometalate were enhanced.
    The Preparation and Biodistribution of a New Potential Myocardial Imaging Agent: Technetium-99m Labeled[Tc(CO)3(TBI)3]+ Complex
    ZHANG Xian-Zhong, WANG Xue-Bin, WEN Hai-Tao
    2003, 24(1):  21-24. 
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    Starting from [99mTcO4]- and at a pressure of 0.1 MPa, the important starting material[99mTc(CO)3(H2O)3] + is synthesized. By ligand exchanging of this starting material with isonitrile ligand TBI (t-butyl-isonitrile), the complex [99mTc(CO)3(TBI)3]+ is prepared with a labeling yield higher than 90%, and it is stable over 6 h at room temperature. The biodistribution of this new complex in normal mice indicates that it is well accumulated and maintained in heart. The values of its heart uptake at 5 and 60 min post-injection time are (19.07±0.81)%(ID/g) and (18.24±2.41)%(ID/g), respectively. The uptake ratios of heart to liver, lung, and blood at 60 min post-injection time are 1.02, 5.83 and 23.69, respectively. Its good properties and easy availability make it a very promising myocardial imaging agent.
    Studies on the Synthesis and RNA Binding of Ruthenium (Ⅱ) Polypyridine Complexes
    XU Hong, DENG Hong, HU Hong-Yu, LIU Jian-Zhong, CHAO Hui, LIU Jie, JI Liang-Nian
    2003, 24(1):  25-27. 
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    A new ruthenium polypyridine complex, [Ru(phen)2(pMIP)]2+(phen=1,10-phenanthroline, pMIP=2-(4-methylphenyl)imidazo phenanthroline), was synthesized and characterized by elementary analysis, MS and 1H NMR. Spectroscopic methods have been carried out on the interaction mechanism of the Ru (Ⅱ) complex with yeast tRNA systematically. The experimental results indicate that the complex binds to yeast tRNA with an intercalative mode possibly, and interacts with yeast tRNA enantioselectively. The experimental results also suggest that spectroscopic method is effective on studying the interaction mechanism of Ru (Ⅱ) complexes with RNA. Information obtained from the study is potentially useful in the design of new RNA-targeting drugs.
    A 3-D Inorganic-organic Hybrid Framework Microporous Material──Synthesis and Characteristic of [Co3(BTC)(HBTC)(H2BTC)(C2H4O2)3]·3(DMF)·6(H3O)
    FANG Qian-Rong, SHI Xin, XIN Ming-Hong, WU Gang, TIAN Ge, ZHU Guang-Shan, LI Ya-Feng, YE Ling, WANG Chun-Lei, ZHANG Zhen-Dong, TANG Lu-Lu, QIU Shi-Lun
    2003, 24(1):  28-31. 
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    Compound [Co3(BTC)(HBTC)(H2BTC)(C2H4O2) 3]·3(DMF)·6(H3O) was synthesized under mild conditions and its crystal structure was determined by using single crystal X-ray diffraction. The crystal structure was solved by direct method and refined by full-matrix least-square method. The crystal is monoclinic and belongs to space group Cc with a=2.645 3(5) nm, b= 1.670 4(3) nm, c=1.821 6(4) nm, β=128.16(3) °, V=6.329(2) nm3, Z=2 , Dc=20.200 Mg/m3, M r= 1 314.744, μ=10.274 mm-1, F(000) =38 226, GOF=0.99, R=0.094 1, ωR=0.257 3.
    Hydrothermal Synthesis and Structural Characterization of a Novel Open-framework Cobalt Phosphate, Co2(HPO4)2·H2O, with 1-D Helical Channels
    ZENG Qing-Xin, CHEN Lian-Shan, LI Ya-Feng, YANG Guo-Yu, XU Ji-Qing
    2003, 24(1):  31-33. 
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    A new Co2(HPO4) 2·H2O has been hydrothermally synthesized firstly. Single crystal X-ray analysis indicates that this compound crystallizes in a hexagonal system, space group P6 5 with a=1.048 31(15) nm, b=1.048 31(15) nm, c=1.496 3(3) nm, α=90°, β=90°, γ=120°, V= 1.424 1(4) nm3, μ=3.849 mm-1, Z=6, F(000)=960, Dc=2.294 g/cm3, R=0.072 1, wR= 0.212 1, S=1.182, Δρmax=1.671×103 e·nm-3 and (Δρ)min=-1.210×103 e·nm-3. Co 1(HPO4)2·H2O is characterized by 1D 12-ring helical channels. Tetrahedral primary structure-building units of CoO4 and PO4 indicates the title compound has a zeotype framework.
    Hydrothermal Synthesis and Crystal Structure of a New Cage-like Isopolyoxovanadate [Ni(1,10′-phen)3]2 [V2V8O26]
    LI Yang-Guang, LUAN Guo-You, WANG En-Bo, WANG Shu-Tao, HU Chang-Wen, HU Ning-Hai, JIA Heng-Qing
    2003, 24(1):  34-36. 
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    A new isopolyoxovanadate [Ni(1,10′-phen)3]2 [V2V8O26] was hydrothermally synthesized and structurally characterized by the single crystal X-ray diffraction. The compound crystallizes in orthorhombic system, space group Pbcn with a=1.362 9(3) nm, b=2.215 6(4) nm, c= 2.571 2(4) nm, V=7.764(2) nm3, Z=4, R=0.040 3, wR2=0.044 6. The compound exhibits an unusual empty ellipsoidal cage, which is constructed by eight {VO4} tetrahedra and two {VO5} square pyramids via corner-sharing modes. The chiral [Ni(1,10′-phen) 3]2+ complexes act as the counter cations.
    Recognition of Thymine by Triazinyl Fluorescence Probe Through the Formation of Intermolecular Multi-hydrogen Bonds
    NIE Li-Hua, MA Hui-Min, LI Xiao-Hua, SUN Ming, YOU Hong-Tao, JIN Yong-Ping
    2003, 24(1):  37-39. 
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    In this work, a novel long-wavelength fluorescence probe, 3-(4-chloro-6-methylamino-1,3,5-triazinylamino)-7-dimethylamino-2-methylphenazine, was synthesized by the reaction of neutral red and methylamine subsequently with cyanuric chloride, and its recognition behavior for thymine together with its spectroscopic properties in different solvents was studied. The results show that the fluorescence probe can be selectively quenched by thymine instead of guanine, suggesting that the fully complementary hydrogen bonding plays a key role in such a recognition process.
    Concentration of Trace Amounts Oligonucleotide Using Super-paramagnetic DNA Nano-enricher
    HE Xiao-Xiao, WANG Ke-Min, TAN Wei-Hong, LIU Bin, LI Du, HUANG Shan-Sheng
    2003, 24(1):  40-42. 
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    The present paper covers a novel technology for the concentration of trace amounts of target oligonucleotide from the solution. This technique is based on a super-paramagnetic DNA nano-enricher constructed with a single strand DNA probe immobilized onto the surface of the super-paramagnetic nanoparticles prepared by using the water-in-oil microemulsion technique, employing silica as the shell and iron oxide as the core of the super-paramagnetic nanoparticles. The silica coated magnetic nanoparticles are (40±4) nm in size. And the magnetic nanoparticle is super-paramagnetic. Biotin labeled ssDNA(Biotin-5-(A)10-GAT-TCA-CGA-GGC-CCT-AGT-CG-3') was immobilized on the surface of silica coated magnetic nanoparticles. The complementary ssDNA could be enriched effectively and the characteristics of the enriched ssDNA have not changed, which will provide a novel technique and measurement for gene transfection, mutation detection, gene diagnosis, gene therapy and so on.
    A Novel Method for the Determination of Nucleic Acids Based on Enzyme Catalyzed Fluorescence Reaction
    WEI Ling, YANG Huang-Hao, CHEN Xiao-Lan, QU Hui-Ying, XU Jin-Gou
    2003, 24(1):  43-45. 
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    A novel fluorimetric method has been developed for the rapid determination of ncleic acids, based on that the catalytic activity of hemin is decreased due to the ion-association with Alcian blue 8GX and recovered when nucleic acids are added to the system. The change in the catalytic activity of hemin results in the fluorescence change of the hemin-catalyzed fluorogenic reaction system of p-hydroxyphenylacetic acid(p-HPA) and H2O2 and the fluorescence change of the system is proportional to the quantities of nucleic acids existing. The corresponding detection limits of the method are 0.91 ng/mL for CT DNA and 7.5 ng/mL for yeast RNA.
    A Novel Capacitive Immunosensor For Direct Detection of Laminine with a Potentiostatic Step
    JIANG De-Chen, TANG Jia, LIU Bao-Hong, SHEN Xian-Rong, ZHANG Song, YANG Peng-Yuan, LI Ai-Zhen, HUANG Yi-Ping, KONG Ji-Lie
    2003, 24(1):  46-48. 
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    Laminine(Ln) has been identified as an important marker of liver fibrosis or cirrhosis. The Ln immunosensor was formed with thioglycolic acid to produce a self-assembled monolayer on the gold electrode surface. The monoclonal Ln antibody was orderly immobilized on the modified gold surface covalently using EDC/NHS. An unlabeled antigen combined on the antibody could reduce the capacitance of the electrode, which was evaluated by the potentiostatic method. The measurement was performed in microseconds. Ln antigen could be determined in the range of 2-50 ng/mL. The quick response made the immunosensor a promising clinical screening method.
    Studies on β-Glucose Chemiluminescence Detection Catalyzed by GOD with Microchip Chemical Reactor
    XU Yi
    2003, 24(1):  49-51. 
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    Glucose oxidization was catalyzed by glucose peroxidase, reactive products peroxides could have Chemiluminescence reaction with luminol. These were applied to detect glucose quantitatively in-situ or on-line by the microreactor with micromixer and FIA system. In this paper, the effects of many factors, such as the characters of microchip, modification of microchip glass surface, pH values of the detecting system, CL intensifying agent and so on, were studied in detail on the glucose detection. A new reliable and portable easily automatable system was set up for the glucose detection.
    Screening of Affinity Peptide Ligands from Combinatorial Peptide Libraries
    FANG Can-Liang, ZHAO Rui, LIU Yang, YU Xiao, XIONG Shao-Xiang, LIU Guo-Quan
    2003, 24(1):  52-54. 
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    A new method for the rapid and efficient screening of affinity ligands to biological targets is reported. The fusion peptide of influenza virus A was used as the model target and immobilized on the PGMA beads. Antisense peptide YRSKQA of fusion peptide was chosen as the lead compound. The special positional scanning peptide libraries were designed based on YRSKQA and synthesized by utilizing solid phase peptide synthesis manually. The libraries were YRSKQX, YRSKXA, YRSXQA, YRXKQA, YXSKQA and XRSKQA, where X represented 18 L-amino acids(except for Cys and Trp). Each library was screened by affinity chromatography. The eluates from the fusion peptide affinity column were collected and analyzed by RP-HPLC and MS, respectively, in order to determine the kind of X at each position. After the preferred residues of six positions were decided, the two preferred peptide sequences, GRGKHK and TRGKHK, were obtained. The dissociation constants of GRGKHK, TRGKHK and YRSKQA, were 3.35×10-6, 5.24×10-6and 1.15×10-5 mol·L-1, respectively. The preferred peptides showed the higher affinity binding to immobilized fusion peptide than the lead peptide.
    Determination of Lead Isotope Ratios in Geological Samples by Inductively Coupled Plasma Mass Spectrometry
    HU Sheng-Hong, YANG Wei, SHUAI Qin, LIU Yong-Sheng, LIN Shou-Lin, GAO Shan
    2003, 24(1):  55-57. 
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    A simple and precise method for direct determination of molar ratio of 206Pb/ 204Pb, 207Pb/ 204Pb and 208Pb/ 204Pb by ICP-MS was developed. The data acquirement parameters of MS for Quadrupole setting time(QST), Dwell time(DT), Integrated time and number of sweeps were investigated in detail. The relative standard deviation(RSD) of different Pb isotope ratios were less than 0.32%[n=5, ρ(Pb)=20 ng/mL]. The mass discrimination and dead time of detector was calibrated by using NIST981 solution. The mass bias factor(α) of 206Pb/ 204Pb, 207Pb/ 204Pb and 208Pb/ 204Pb were 0.002 5, 0.002 9 and 0.002 0, respectively. The dead time of detector was 7 ns. The proposed method has been applied to the analysis of geological standard reference materials containing AGV-1, BCR-2 and BHVO-2 .The relative error between this work and the recommend values or reported values was better than 0.73% and the relative standard deviation was better than 0.93%(n=5).
    Synthesis and Crystal Structure of 2,3,4,6-Tetra-O-acetyl-(β-D-glycosyl)-isothiocyanate
    JIAN Fang-Fang, WEN Li-Rong, LI Xue-Mei, ZHANG Shu-Sheng, JIAO Kui
    2003, 24(1):  58-60. 
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    The title compound, 2,3,4,6-tetra-O-acetyl-(β-D-glycosyl)-isothiocyanate( C15H27·NO9S), were synthesized and its crystal structure was characterized. It crystallizes in cubic system, space group P212121 with the cell parameters a=1.294 3(3) nm, b=0.828 40(2) nm, c=1.514 8(3) nm, V=1.623 9(6) nm3, Z=4. The hexopyranosyl ring adopts a normal 4C1 chair conformation with total puckering amplitude, QT of 0.606.
    New Sucrose Esters from Securidaca Inappendiculata
    YANG Xue-Dong, LIU Jiang-Yun, XU Li, XU Li-Zhen, YANG Shi-Lin
    2003, 24(1):  61-63. 
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    Three sucrose esters, β-D-(3,4-O\%-disinapoyl)fructofuranosyl-α-D-(6-O-sinapoyl)gluco-pyranoside(1), β-D-(3-O-feruloyl)fructofuranosyl-α-D-(6-O-sinapoyl)glucopyrano-side(2), and β-D-(3-O-feruloyl) fructofuranosyl-α-D-(6-O-feruloyl)glucopyranoside(3) were isolated from the stems of Securidaca inappendiculata collected from Yunnan Province. Among them, compound 3 was a new sucrose ester and was named as securoside A . All structures were elucidated on the basis of chemical and spectroscopic evidence, especially 13C, 1M NMR and ESI-MS experiments.
    Selective One-pot Synthetic Method for Imidazole and Benzimidazole Derivatives
    JIANG Zong-Lin, XIAO Rong, SU Xiao-Yu, YAN Jia-Ming, XIE Ru-Gang
    2003, 24(1):  64-67. 
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    A novel and selective one-pot synthetic method of imidazole and benzimidazole derivatives has been developed. Three series of target compounds, 1-(ω-haloalkyl) imidazoles 3a-3e, bis-imidazoles 5a-5b and tri-imidazoles 6a-6b have been synthesized by the selective quaterisation of 1H-imidazole-1-propanenitrile (1) with α, ω-dihalide, bis(bromomethyl) benzene or tri(bromomethyl) benzene to obtain imidazolium salts, following by Hoffmann-type elimination. Similarly, benzimidazole analogues 7 and 8 were also prepared. It is found that important factors affecting this selective quaterisation are the solvent, temperature, structure and amount of halides.
    Synthesis and Structure of Seven-coordinate Dimer {(PhCH2)2Sn[2,6-(O2C)2C5H3N](CH3OH)}2
    YIN Han-Dong, WANG Chuan-Hua, WANG Yong, MA Chun-Lin, SHAO Jian-Xin
    2003, 24(1):  68-72. 
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    A novel seven-coordinate dimer {(PhCH2)2Sn[2,6-(O2C)2C 5H3N](CH3OH)}2 was synthesized by the reaction of(PhCH2)3SnCl with 2,6-pyridine dicarboxylic acid in 1:1 molar ratio in methanol with Et3N. The structure of the dimmer was characterized by elemental analysis, IR, 1H NMR, and X-ray single crystal diffraction. The crystal belongs to a triclinic system with space group P1, a=0.962 5(6) nm, b=1.094 7(9) nm, c=1.996(3) nm, α=90.00(2)°, β=87.69(3)°, γ=90.00(3)°, Z=2, V=2.102(6) nm3, μ=1.248 mm-1, F(000)=1 000, R1=0.047 6, wR2= 0.078 2. In the crystals of complex, the tin atoms rendered seven-coordinate in a distorted pengonal bipyramidal structure. The complex was tested in vitro against human tumour cell lines, MCF-7 and WiDr, and displayed a higher activity.
    A Kinetic NMR Study of Reduction Mechanism of NADH Models
    LI Jing, LIU You-Cheng, WU Sai-Yu, XIA Jing-Jing, ZHANG Jia-Hai, WU Ji-Hui
    2003, 24(1):  73-75. 
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    The rate constant and kinetic isotopic effect(kH/kD) of the reduction of 2-bromo-1-phenylethylidenemalononitrile with NADH model were determined through NMR spectroscopy. The results were consistent with that the hydride transfer step of the reaction which was the rate-determining step, and were comparable to the results obtained through UV-Vis Spectroscopy reported previously.
    Asymmetric Epoxidation of Olefins Catalyzed by Chiral Iminium Salts Generated in situ from Chiral Amines and Aldehydes
    ZHENG Yan-Song, JIANG An
    2003, 24(1):  76-78. 
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    Asymmetric epoxidation of olefins with oxone was first catalyzed by chiral iminium salts generated in situ from chiral amines and aldehydes. With 2S,5S-2,5-dicyclohexylaminocarbonylpyrolidine and t-butylacetaldehyde, trans-stilbene were epoxdized in 80% conversion, 93% yield and 65% e.e. at 0 ℃.
    A Novel One-pot Synthesis of 3,4-Dihydropyrimidine-2(1H)-ones Catalyzed by Indium Tribromide
    FU Nan-Yan, YUAN Yao-Feng, PANG Mei-Li, WANG Ji-Tao
    2003, 24(1):  79-81. 
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    A novel catalyst indium(Ⅲ) tribromide is shown to efficiently promote 5-carbonyl-4-aryl-3,4-dihydropyrimidin-2(1H)-ones from a three-component coupling of β-diketones, aldehydes and urea in ethanol. This modified one-pot Biginelli′s cyclocondensation not only features simple operation, but also takes place in nonpolluted environment. The structure of the Biginelli reaction product from β-diketones, salicylaldehyde and urea has been proposed to possess an oxygen-bridge.
    Synthesis of New Phase ZnO Nanoparticles Under Room Temperature and Characterization
    YANG Qing-Lin, GUO Lin, WU Zhong-Hua, JIANG Lei, XU Wen-Guo, LI Qian-Shu
    2003, 24(1):  82-85. 
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    In the present research, we report the synthesis of ZnO nanoparticles modified by polyvinyl pyrrolidone(PVP). The resulting ZnO has the mean diameter of 4.0 nm with the narrow distribution. It has the same structure phase with bulk ZnO which is synthesized under 450 ℃, 6×108 Pa preparation condition. The EXAFS results reveal that with the decrease of ZnO particle sizes to the nanometer range the coordination number decrease. The interaction between oxygen and Zinc is relatively stronger in these nanosized materials, the Zn-O bond length is slightly shorter than one in the bulk ZnO indicating a structural contraction for the small nanoparticles.
    A New Technique of the Characterization of Monolayers on Silicon Surfaces──Measure of the Differential Capacity of Interfaces
    SUN Qiao-Yu, Henry de Villeneuve Catherine, LI Hu-Lin, Allongue Philippe
    2003, 24(1):  86-90. 
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    We suggest a new technique to characterize the organic monolayers on silicon surfacesmeasurement of the differential capacity-electrode potential curve. By means of the investigation of differential capacity of a series of alkenes-modified silicon surfaces and H-Si(111)/electrolyte interfaces, we have established the relationship between the structure of the organic monolayers on silicon surfaces and their interface differential capacity. It has been confirmed to be a simple, quick, and effective experimental technique for the research of chemical modifications and functions on the silicon surfaces.
    Microcalorimetric Study of the Associated Action of Selenium to Arsenic on the Growth of Escherichia coli
    LI Xi, LIU Yi, WU Jun, QU Song-Sheng
    2003, 24(1):  91-94. 
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    Escherichia coli was used as an experimental object, the associated action between selenomorpholine and sodium arsenite was studied by microcalorimetry. The experiment results showed that there was antagonistic or cooperative interaction between selenomorpholine and sodium arsenite, and whether antagonistic or cooperative interaction between selenium and arsenic depended on their relative concentrations. The mechanism of the associated action between selenomorpholine and sodium arsenite perhaps is due to the synthesis of the enzyme in the growth of the bacteria.
    Studies on the Preparation of Alumina Supported on Carbon Nanotubes and Defluorination from Absorbed Water
    WANG Shu-Guang, LI Yan-Hui, ZHAO Dan, ZHAO Hua-Zhang, XU Cai-Lu, LUAN Zhao-Kun, LIANG Ji, WU De-Hai
    2003, 24(1):  95-99. 
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    A novel material for fluoride removal, alumina supported on carbon nanotubes (Al2O3/CNT), was prepared from carbon nanotubes and aluminium nitrate. X-ray diffraction(XRD) spectra demonstrate that alumina was amorphous at calcination temperature lower than 850 ℃ while it was α-Al2O3 at 1 050 ℃. Scanning electron microscope(SEM) images showed that the CNT and alumina were homogenously mixed. Furthermore, the fluoride adsorption behavior on the surface of Al2O3/CNT was investigated. The results indicated that Al2O3/CNT had a high adsorption capacity. The fluoride adsorption capacity of the Al2O3/CNT, which was prepared under the conditions of 450 ℃ calcination temperature and 30% Al2O3 supported, was 2.0-3.5 times that of γ-Al2O3 and almost equals to that of IRA-410 polymeric resin. The adsorption isotherms of fluoride on Al2O3/CNT fit the Freundlich equation well, and optimal pH ranging from 5.0 to 9.0.
    Desulfurization and Kinetic Studies on CaCO3-SiO2 Complex Desulfurization Reagent
    GUO Feng, WU Zeng-Hua, CUI Ai-Li, WANG Li-Xin
    2003, 24(1):  100-104. 
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    In this paper, Ca-Si complex desulfurization reagent was prepared by precipitation, sol-gel and mixing method. Then the effect on desulfurization among differet samples was studied. The grain model of the reaction kinetic was used. It is shown that this model can describe the course of desulfurization. Different samples have different effects on the kinetic parameter such as Ea and k0, which couple to each other(the accretion of Ea always accompanies the accretion of k0 and vice versa). The sol-gel-Ca-Si reagent gives the best performance on desulfurization. At the beginning of the reaction, the complex Ca-Si reagent shows the slow rate, but in the end, it is obviously faster, further more, the higher the temperature of the reactions, the greater the effect.
    Theoretical Studies on the Structures and Stability of C40 Isomers
    LIU Gui-Xia, ZHANG Hong-Xing, SUN Chia-Chung, TANG Ao-Qing
    2003, 24(1):  105-108. 
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    The Becke-3-Lee-Yang-Parr(B3LYP) method and 6-31G basis set was employed to study the equilibrium geometries and electronic structures of six kinds of C40 fullerene isomers, i.e., the isomers with D5d, Td, D2h, C3v, D2(Ⅰ) and D2(Ⅱ) symmetries. Due to the Jahn-Teller distortion we calculated the D2d(Td) structure in stead of Td strucure of C40. Mealwhile, the stability order of the six kinds of C40 isomers was judged from the total energies of them.According to our calculations, the stability order is D2(Ⅰ)>D5d>D2d(Td)>C3v>D2h>D2(Ⅱ), which is in good agreement with Salcedo et al.′s computational result of D5d>D2d>D2h at the HF/3-21G level, and is consistent with Zhang et al.′s proposal that the D2(Ⅰ) structure of C40 isomers is the most stable one. In addition, our calculated results also confirmed that the HOMo-LUMO gap is not reliable to predict the stability of fullerenes.
    Theoretical Studies on Two Reactions of 1-Trichlorostannylbuta-2,3-butadiene and 2-Trichlorostannylbuta-1,3-butadiene with Formaldehyde by B3LYP
    XIA Lu-Hui, XU Kai-Lai, LUO Mei-Ming, FANG De-Cai, XIE Dai-Qian
    2003, 24(1):  109-112. 
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    The two reactions of 1-trichlorostannylbuta-2,3-butadiene and 2-trichlorostannylbuta-1,3-butadiene with formaldehyde have been studied by using the density functional method at the B3LYP/6-31G ** level. The structures and energies of the stationary points were calculated to produce the activation barriers, free energy changes and equilibrium constants. The transition states were testified by using vibration analysis and IRC calculations. The two reactions in CH2Cl2 solvent at 1.013×105 Pa and 298.2 K have also been studied by the SCRF(PCM) method at the same level. The results show that the reactions take place with high regioselectivity and mainly produce the product of the reaction of the 1-trichlorostannylbuta-2,3-butadiene with formaldehyde.
    Theoretical Studies on Structures and Properties of (NO)2+ Complex Cation
    SUN Li-Xiang, BU Yu-Xiang, CHEN Zhi-Da
    2003, 24(1):  113-116. 
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    The NO dimer cation, (NO)2+, has been studied by using density functional theory. The geometries and the harmonic vibrational frequency of (NO)2+ have been calculated at B3LYP/ 6-311++G* level. The results indicate that there are five stable doublet states. The ground state is determined to be the trans isomer with N-N bond linkage, which has C2h symmetry. The relative stability of all stable geometric structures has been analyzed. The state-state correlation and the isomerization mechanism are predicted by searching the transition states and using the same methods.
    Preparation, Structure and Properties of Microencapsulated Alginate Ionotropic Gels
    CHEN Yi-Qing, SUN Duo-Xian, LIU Jing-Yi, Lü Jing-Hui
    2003, 24(1):  117-120. 
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    The microencapsulated alginate ionotropic gels[alginate-chitosan-alginate(ACA) microcapsules, a kind of novel ion adsorbents] are prepared and employed to examine their ion exchange properties. FTIR spectra reveal that ACA has a capsular structure composed of capsular membrane with alginate-chitosan polyelectrolyte complex and intracapsular alginate solution. ACA microcapsules particle sizes are about 400-450 μm, its smooth surface and clear capsular membrane was observed by optical microscope. The membrane thickness is 8-10 μm determined by SEM. The SEM analysis proves that the process of adsorption of ACA on heavy metals is sol-gel transition process and the process of desorption of ACA on heavy metals is gel-sol transition process. So ACA is a kind of ionotropic gels. As novel ion adsorbents, ACA microcapsules have a higher percent adsorption, lower limiting adsorption concentration, higher enrichment capacity than usual ion exchange resins on Pb2+. The highest percent adsorption is 99.90%. The limiting adsorption concentration is 0.021 6 mg/L. The weight exchange capacity is 311 mg(Pb)/g at an equilibrium concentration of 1.5 mmol/L Pb2+ ions. Especially ACA microcapsules have much faster ion exchange velocity than D418 chelating resin and D113 polyacrylate resin in the controlled experiments. The mutual diffusion of metal ions and alginate molecules decreases the diffusion distance of exchange ions and increasingly enhances ion exchange velocity. At last, it is proved that ACA can be used for many times.
    Selective Hydrogenation of Acetic Acid to Acetaldehyde over SBA-15 Supported Iron Oxide Catalysts
    ZHANG Xue-Zheng, YUE Ying-Hong, GAO Zi
    2003, 24(1):  121-124. 
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    A series of SBA-15 supported α-Fe2O3 catalysts were prepared and characterized. The influence of iron oxide loading, reduction temperature and reaction temperature on the catalytic activity and selectivity for the selective hydrogenation of acetic acid to acetaldehyde was investigated. The highest yield of acetaldehyde over the supported catalysts is 42.7%, whereas that over non-supported α-Fe2O3 is only 32.2%. The hydrogenation catalysts need to be prereduced before reaction. The optinum reduction temperatures for α-Fe2O3 and the supported catalyst are 873 and 923 K, respectively. The selective hydrogenation to acetaldehyde is favored when Fe3O4 and Fe0 coexist on the catalyst surface, and acetaldehyde is likely formed via a Mars-van Krevelen reaction mechanism.
    Preparation and Characterization of Supported Catalyst Sn2(OMe)2Cl2/SiO2 and Its Catalytic Properties for Synthesis of Dimethyl Carbonate
    ZHONG Shun-He, CHENG Qing-Yan, LI Han-Sheng
    2003, 24(1):  125-129. 
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    Silica supported binuclear bridged complex Sn2(OMe)2Cl2/SiO2 was prepared by surface modification. IR, TPD and micro-reactor evaluation techniques were used to characterize the surface structure, absorption properties and reactivity of Sn2(OMe)2Cl2/SiO2. The results indicate that the Cl-is the ligands of Sn2(OMe)2Cl2/SiO2 , bis-μ-OMe bridged Sn2(OMe)2 can be formed between the two Sn4+metal ions and bonded on the surface of SiO2 by Sn-O-Si bonds; CO2 can be chemisorbed on Sn2(OMe)22/SiO2 catalyst to form bridged adsorption state and methyl carbonate species, CH3OH can be chemisorbed on the catalyst to form molecular adsorption state. At the reaction temperature 413 K, the Sn2(OMe)2Cl2/SiO2 catalyst has almost 100% DMC selectivity for DMC direct synthesis from CO2 and CH3OH. The mechanism for DMC synthesis from CO2 and CH3OH on the surface of Sn2(OMe)2Cl2/SiO2 is proposed based on the experimental results. The reactants CO2 and CH3OH co-adsorbing at the same active site on the surface of Sn2(OMe)4/SiO2 and the formation of methoxy carbonate species of CO2 on the surface of the catalyst were the critical steps for the DMC synthesis.
    A Study on n-Pentane Reactions over Peroxodisulfated Zirconia and Sulfated Zirconia Solid Superacid
    SONG Guo-Xin, WANG Lin, XUE Hua-Xin, ZHANG Li, CHEN Jian-Min
    2003, 24(1):  130-134. 
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    n-Pentane reaction over S22-82(PSZ) at an ambient temperature in the steady state system has been introduced in relation with the same reaction occurring over SO2-4/ZrO2(SZ). It can be concluded that both PSZ and SZ have two functions on n-pentane: isomerization and cracking. The products of the two reactions are i-pentane and i-butane respectively. The conversion of n-pentane isomerization and apparent reactive velocity constant lie mainly on the calcining temperature of each sample. The catalysis activity of PSZ is higher than that of SZ: the molar ratio of i-pentane over the former to that over the latter is 1.3/1 after 1 h reaction. The optimum calcining temperature of PSZ is 550 ℃, which is 50 ℃ lower than that of SZ. By means of S-content measurement, BET, XRD, FTIR and chemical analysis, the physical and chemical characteristics of S22-82 can be attained. We draw a conclusion that PSZ has stronger Lewis acidic sites and more acid quantity than SZ from the results of the in situ FTIR and Pyridine-FTIR experiment.
    Studies on the Photo Stimulated Surface-catalytic Reaction of Carbon Dioxide and Water over Cu/ZnO-NiO
    CHEN Song-Zhe, ZHONG Shun-He
    2003, 24(1):  135-139. 
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    The n-p coupled semiconductor material 0.5%Cu/ZnO-1.5%NiO was prepared by using sol-gel method, over which the photo stimulated surface-catalytic reaction(PSSR) of synthesis of CH3OH from CO2 and H2O was studied. XRD, TEM, IR, UV-Vis and TPD experiments were adopted for characterizing the structure, photon absorbing and chemisorbing ability of the material. It was revealed that, during PSSR over the prepared material, CH3OH, CH4 and CO can be secured at a normal temperature. The influence of temperature on PSSR was discussed, based on which shearing and horizontal chemisorption states of CO2 were ascertained to be the surface precursors of CH4 and CH3OH, respectively. Finally the PSSR mechanism was presented.
    A Novel Preparation for a Self-humidifying Membrane Electrode Assembly and Performance of Its Fuel Cell
    WANG Cheng, MAO Zong-Qiang, XU Jing-Ming, XIE Xiao-Feng
    2003, 24(1):  140-142. 
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    A novel method for the preparation of a self-humidifying MEA used for PEMFC and the optimum conditions for the fabrication are presented. Different from the method involved dispersion of Pt particles through out the membrane or between two thin membranes. The new type self-humidifying MEA gain self-humidifying operation by asymmetry electrode. The anode with 0.1 mg Pt/cm2, has super-hydrophilicity by coating the hydrophilic colloid, while the cathode with 0.4 mg Pt/cm2, has a strong hydrophobic nature by doping PTFE. When the current density is less than 2.3 A/cm2, the discharge performance of the humidifying gases little excel the self-humidifying operation, but more than 2.3 A/cm2, the self-humidifying operation do better than humidifying gases operation, and the most power density reaches over 1.5 W/cm2. Inner resistance of electrochemistry reaction and transportation are studied by the AC impedance method, and validate that the self-humidifying MEA can give a good three-dimension reaction area with dry hydrogen and dry oxygen.
    Preparation of Azophenyl-substituted Pyrazoline Derivatives and Studies on Photoinduced Birefringence of Doped PMMA Films
    JIN Ming, YANG Qing-Xin, LU Ran, PAN Ling-Yun, ZHAO Ying-Ying
    2003, 24(1):  143-145. 
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    Three azo-dyes, 4′-{[(2-hydroxylethyl)methyl]amino}-4-nitroazobenzene(1), 1-[4-(4′-nitrophenyl)-azophenyl]-3,5-biphenyl-2-pyrazoline(2) and 1-[4-(4′-nitrophenyl)-azophenyl]-5-(4′-hydroxylphenyl)-3-phenyl-2-pyrazoline(3) were synthesized. The polarized photoinduced birefringence and relaxation process of those azo-dyes doped with PMMA films were investigated under polarized laser intensity. The results indicate that compounds with pyrazoline group have a high storage rate and thermal stability. It has been found that the birefringence signals decrease with the increase of the temperature, but the effect of temperature is different for the three compounds. Compounds 2 and 3, with pyrazoline groups have a good thermal stability at room temperature, and compound 3 can even keep 30% of its maximum birefringence at 90 ℃.
    Surface Texture of Nanometer Mesoporous Titania Powders
    YANG Ru, LI Min, LI You-Fen, LIU Jia-Xiang, YAN Cai-Xia
    2003, 24(1):  146-150. 
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    Nanometer titania mesoporous powders were prepared by heating the mixed solution of titanium disulfate and polyethylene glycol(PEG-1000) in the presence of urea under hydrothermal conditions at 104 ℃.The texture, morphology and crystallite size of the synthesized nanoparticle powders were investigated by XRD, BET, TEM and DSC. The powders dried at room temperature and calcined at temperature below 850 ℃, their particles were spherical, well dispersed, ultrafine titania, with anatase phase. Their crystallite size increased from 8.56 to 48.82 nm with increasing the calcining temperature from room temperature to 850 ℃.The pore structure among particles, open-ended tubular pores, were mesoporous texture, the average pore diameters were from 10.36 to 27.25 nm.
    The Glass Transition of Copolyester
    BIAN Jie, YE Sheng-Rong, FENG Lin-Xian
    2003, 24(1):  155-159. 
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    The glass transition of poly(ethylene tetrephthalate/isophthalate) and poly-(ethylene/teramethylene tetrephthalate) copolyesters were studied by using DSC,DLI (depolarized light intensity) and IR analysis. It was shown that the glass transition of copolyesters was a change after the disorientation of the order in their glassy state. The forms of glass transition in DSC thermograms of the two serial copolyesters transformed from step change to endothermic peak with the increase of ET segments in the molecular chains. This is caused by the decrease in the number of ET segments which need to maintain their conformation change. The order of glassy P(ET/EI) copolyester relates to the free hydroxy at the end of the chains. The formation of hydrogen bond between free hydroxy and carbonyl is a necessary process when PET and crystallizable copolyester crystallizing, and the glass transition of uncrystallizable copolyester(IPA 30) will disappear after the formation of these hydrogen bonds.
    The Self-assembly Behavior of PS-PMMA/PMMA in Selective Solvents
    YIN Fen-Fang, SHI Lin-Qi, AN Ying-Li, ZHANG Wang-Qing, HE Bing-Lin, GUO Shi-Yi
    2003, 24(1):  160-164. 
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    The self-assembly of PS-PMMA/PMMA in selective solvents was studied by dynamic laser light scattering(DLS) and transmission electron microscope(TEM). The selective solvent was the good solvent for PS block while it was a precipitant for PMMA block and homopolymer. The results showed that the PS-PMMA/PMMA with a proper molecular weight and composition could self-assemble into micelles with mono-dispersity distribution. The homopolymer(PMMA) could assemble into the core of the micelles by a special interaction with the block PMMA and accelerate the process of the micellization. The micelles with different sizes can be obtained conveniently by adjusting the content of the homopolymer.
    Synthesis and Characterization of a Novel Photo Alignment Layer for Liquid Crystal Based on Epoxy
    YU Hai-Feng, BAI He, LIAN Yan-Qing, WANG Xiao-Gong, LIU De-Shan
    2003, 24(1):  165-168. 
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    The precursor EP-AN was synthesized by means of the polymerization between aniline and Biphenol-A epoxy which is industrial products. Then the cinnamate groups were attached to the chains of the hydroxyl-containing precursor to prepare EP-AN-CI, which is the potential photo alignment layer for liquid crystal. They were characterized by 1H-NMR, FTIR, and differential scanning calorimetry(DSC). EP-AN-CI was spin-coated on a ITO glass substrate from chloroform solution, resulting in a thin film, then though the linearly polarized polymerization(LPP) it was changed into photo alignment layer. LC cells of a 10 μm-thick were assembled via a capillary action. The photomocrographies were obtained which can be used to explain that EP-AN-CI can be applied in photo alignment layer.
    Intercalation and Assembly of Supramolecular Materials of Glutamic Acid Pillared Layered Double Hydroxides
    REN Ling-Ling, HE Jing, EVANS David G., DUAN Xue 
    2003, 24(1):  169-173. 
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    Glutamic acids were intercalated into the layered double hydroxides by a new synthesis method, from which high crystallized supramolecular materials were obtained and glutamate acids were ordered between layers without carbon dioxides. The structures of supramolecular materials were characterized by powder X-ray diffraction, atom absorbed spectra, FTIR spectra and thermal analysis and the structure models were given out.
    A Multilayer Langmuir-Blodgett Film of Reversed Duckweed Polymer ES-3 Studied by Infrared Grazing Reflection-absorption Spectroscopy
    WANG Qiang, XU Wei-Qing, ZHAO Bing 
    2003, 24(1):  174-177. 
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    Molecular orientation and phase transition behavior in the multilayer Langmuir-Blodgett(LB) film of reversed duckweed polymer ES-3 were investigated by infrared grazing reflection-absorption(IR-GRA) spectroscopy. It was found that the orientation of alkyl chains was nearly perpendicular to the substrate surface for ES-3 LB film on Au-evaperated glass slide. The study on its thermal transition behavior indicates that ES-3 LB film has three phase transition processes,occurring near 65, 105 and 140 ℃, respectively. The first transition corresponds to a conversion from a highly ordered state to the slightly less ordered one with a little increase in the mobility of alkyl chains; the second process is attributable to the order-disorder transition of alkyl chains; and the third is a process of collapse of layer structure.
    Encapsulating of Aqueous CdTe Nanocrystals into Polymerizable Surfactants
    ZHANG Hao, LU Guang, JI Xiu-Lei, LI Zhe, YANG Bai
    2003, 24(1):  178-180. 
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    A variety of polymerizable surfactants were used for aqueous CdTe nanocrystals encapsulation. The luminescent intensity and the solubility of surfactants encapsulated with CdTe nanocrystals can be tailored by choosing the surfactants with different hydrocarbon chain lengths. The ability to encapsulate different color emission nanocrystals with polymerizable surfactants gives great promise for the fabrication of transparent bulk nanocrystal-polymer hybrids.
    Covalent-attached Self-assembly Film Based on Diazoresin and Bovine Serum Albumin and the Cell Culture on Its Surface
    FU Yin, YAO Gui-Jun, DONG Yu-Ping, CAO Yu-Jing, DUAN En-Kui
    2003, 24(1):  181-183. 
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    A novel multilayer film was fabricated from bovine serum albumin(BSA), as polyanion through the adjusting of pH value (pH=7.0), and photo-sensitive diazoresin (DR), as polycation (pH=6.5), in aqueous solution via electrostatic self-assembly. The results show that the absorbance at 383 nm characterized of diazonium group of multilayer films increased with the increase of bilayer number. A good linear relationship between absorbance at 383 nm and the bilayer number indicates that a smooth step-by-step fabrication has taken place on the quartz wafer. Under UV irradiation, following the decomposition of diazonium group between the adjacent interfaces of the multilayers, the ionic bonds of the self-assembly film were converted to covalent bonds and the film becomes very stable toward electrolyte aqueous solutions. Due to the cellular affinity of serum albumin, uterine epithelial cell monolayer was successfully cultured on the surface of self-assembled film of DR/BSA.
    Synthesis of Fluorine-containing Poly(aryl ether) with Low Dielectric Constant
    HU Wei, LIU Bai-Jun, ZHANG Li-Mei, ZHANG Shu-Ling, JIANG Zhen-Hua, WANG Gui-Bin, WU Zhong-Wen
    2003, 24(1):  184-185. 
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    A kind of high Fluorine-containing poly(aryl ether) without side reaction was synthesized in a two-step synthesis. Its structure was confirmed by FTIR, 1H NMR and 19F NMR. The polymer shows an excellent thermal stability, good solubility, low water absorption, low dielectric constant and low refractive index. Flexible and transparant thin film can be easily obtained by compression moulding or solution casting. The polymer would be a promising material used for microelectronics and waveguide devices.
    Synthesis and Characterization of Photopolymerized Supramolecular-structured Hydrogels of α-CD Assemblies
    ZHAO San-Ping, FENG Zeng-Guo, PIAO Dong-Xu
    2003, 24(1):  186-188. 
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    In this paper, the polypseudorotaxanes were synthesized from α-cyclodextrins(α-CDs) threaded onto PCL-PEG-PCL macromers terminated with acrylate groups. Then, supramolecular-structured hydrogels were prepared from the polyseudorotaxanes in a mixed solvent of H2O and DMSO via in-situ polymerization photoinitiated under UV. The structure and properties of the supramolecular-structured hydrogels were characterized by FTIR, TGA and WAXD. The results showed that α-CDs were threaded and immobilized on the network of the hydrogel by rapid photopolymerization, and the feed ratio of α-CDs affected the structure of hydrogels, water absorption, the distribution and states of water, etc..