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Table of Content

    24 June 2002, Volume 23 Issue 6
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    Articles
    Studies on Trans-human Red Cells of Rare Earth Ions by Fura-2 Indicator
    YANG Pin, WEI Chun-Ying, CHEN Juan
    2002, 23(6):  985-990. 
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    The transmembrane behavior of La3+ and Eu3+ was examined by using Fura-2 technique. The result showing a low concentration La3+ or Eu3+ (5×10-6mol/L) could not enter fresh and ATPdepleted human red cells. But in the presence of ionomycin, obvious transmembrane phenomenon was observed when La3+ (or Eu3+)of 5×10-6mol/Lwas added. KCl and Bay K8644 could not promote the influx of La3+ (or Eu3+). Moreover, a low concentration La3+ (or Eu3+) had no effect on the influx of Ca 2+ in ATPdepleted human red cells. When a higher concentration La3+ or Eu3+ (5×10-4mol/L) was added, red cells became hemolysis. Acharacterization of La3+ (or Eu3+)-Fura-2 interactions showed that they formed a 1∶1 La3+ (or Eu3+)-Fura-2 complex. In vitro studies confirmed that Fura-2 fluorescence was sensitive to La3+ (or Eu3+) and the apparent dissociation constants of La3+ and Eu3+ for Fura-2 (Kd) were 1.7×10-12 and 4.95×10-14mol/L, respectively (pH=7.05).
    Synthesis, Crystal Structure and Antibacterial Activity of Copper(Ⅱ) Complexes with 2-oxo-Propionic Acid Salicyloyl Hydrazone
    HE Shui-Yang, CAO Wen-Kai, CHEN Jun-Li, ZHAO Jian-She, SHI Qi-Zhen
    2002, 23(6):  991-995. 
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    Two copper(Ⅱ) complexes with 2-oxo-propionic acid salicyloyl hydrazone, Cu(C10 H8N2O4)·(H2O)2 (1) and Cu(C10 H8N2O4)(CH3OH)(H2O) (2) (C10 H8N2O42- is the dinegative ion of 2-oxo-propionic acid salicyloyl hydrazone), have been synthesized. Bottle green prismatic crystals of complex 2 were obtained, and the crystal structure was determined by single crystal X-ray diffraction. Complex 2 crystallized in the triclinic space group P1 with a=0.7538(2) nm, b=1.1431(2) nm, c=0.7500(2) nm, a=93.26(2)o, β-=94.46(2)o, γ =94.39(2)o, V=0.6411(2) nm3, μ =1.731 mm-1, Z=2, Dc=1.792 g/cm3, F(000)=342.00, GOF=1.78, R=0.035, wR=0.048 for 2630 observed reflections [ I>3.00σ(I)] out of 2946 unique reflections. In complex 2, Cu atom is square pyramidally coordinated by two Oatoms and one Natom of tridentate C10 H8N2O42- ligand, one Oatom of methanol molecule and one Oatom of water molecule with the Oatom of methanol molecule locating at the apical position. The crystal of complex 2 is a racemic compound, included a couple of enantiomers. The couples of enantiomers occur in the crystal of complex 2 in dimer bonding with two hydrogen bonds. According to elemental analyse and IR, the structure of complex 1 is supposed to be similar to that of complex 2. The results of biological activity tests show that complex 1 has 100% and 66.02% of bacteriostastic activity for phytophthora capsic and alternaria alternaea, respectively.
    Isolation and Characterization of the Endohedral Metallofullerene Tb3N@C80
    FENG Lai, XU Jian-Xun, SHI Zu-Jin, HE Xiao-Ran, GU Zhen-Nan
    2002, 23(6):  996-998. 
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    The endohedral metallofullerene Tb3N@C80 was synthesized by using an improved DCarc discharge method under a He atmosphere containing 2%～5% nitrogen. The experimental results indicated that the introduction of small amounts of nitrogen into the electric arc reactor led to the production of Tb3N@C80. The technique of high pressure and high temperature extraction with DMFand two step HPLCmethod were used to extract and isolate small amounts of Tb3N@C80. The sample was characterized by HPLC, MALDI TOFmass spectrum and UV-Vis-NIRspectrum. The observed isotope distribution is consistent with the expected isotope distribution for Tb3N@C80, which shows that the sample obtained should be Tb3N@C80. The UV-Vis-NIRspectrum shows a large difference between Tb3N@C80 and M@C82 (M=Tb, Gd, La and so on).
    Axial Coordination Between Nematic Liquid Crystal 5CB and Fe(Ⅲ) Porphyrins
    LI Tao, HUANG Jin-Wang, HU Shu-Guang, PENG Xiao-Bin, LIANG Dong, JI Liang-Nian
    2002, 23(6):  999-1001. 
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    The axial coordination between nematic liquid crystal 5CBand iron(Ⅲ) porphyrins with different coordination properties was studied by the magnetic field induced Freedericksz Transition and UV-Vis spectra. The results indicated that 5CBdoped with five coordinated Fe(TPP)Cl dramatically decreased the critical magnetic field and the Soret band of Fe(TPP)Cl doped in 5CBhad red shift to some extent. These are resulted from the axial coordination between 5CBand five coordinated Fe(TPP)Cl.
    Hydrothermal Synthesis and Crystal Structure of a Novel 3-D Compound [H0.5CoP0.5O2.5]
    LI Chuan-Bi, XU Ji-Qing, ZENG Qing-Xin, SU Chang, ZHANG Li-Juan, YE Ling
    2002, 23(6):  1002-1003. 
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    Anovel 3-D compound, [H0.5CoP0.5 O2.5], was hydrothermally synthesized and structurally characterized by singly crystal X-ray diffraction, ICP, elemental analysis and IRspectra. The compound crystallizes in orthorhombic system, space group Pnnm with a=0.8051(2) nm, b=0.83809(13) nm, c=0.5950(2) nm, V=0.401(2) nm3, Z=1, D=1.669 Mg/cm3, R=0.0491, wR=0.1532.
    Synthesis, Structure and Stability of Binuclear Metal Complexes with Macrocyclic Ligand
    CHEN Shi, LU Tong-Bu, FENG Xiao-Long, LI Yan-Wu, MAO Zong-Wan, JI Liang-Nian
    2002, 23(6):  1004-1006. 
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    The macrocyclic ligand(L) and its dinuclear copper(Ⅱ) and zinc(Ⅱ) complexes have been synthesized. The crystal structure of [Cu 2L(Him)2](ClO4)4·2H2O has been determined by single crystal X-ray diffraction. It crystallizes in a monoclinic system, the space group P2 1/c, a=0.9512(2) nm, b=2.0104(4) nm, c=1.2025(2) nm, β-=98.89(3)°, V=2.2719(8) nm3, Z=2, Dc=1.599 Mg/m3, F(000) = 876, R=0.0591, wR=0.1733, GOF(F)=1.009. The copper(Ⅱ) atom is five coordinated with four nitrogen atoms of the macrocyclic ligand and one nitrogen atom of imidazole. The stepwise stability constants of the 1∶1 and 2∶1 molar ratios of Cu to Land Zn to Lcomplexes were determined by potentiometric titration in KCl supporting electrolyte(0.100 mol/L) at 25 ℃. The results indicated that zinc(Ⅱ) ion can form hydroxide bridged dinuclear complex [Zn2(OH)L]3+, while the copper(Ⅱ) ion can only form dinuclear complex [Cu2L]3+ with macrocyclic ligand.
    Synthesis and Characterization of Complex η2-C60[Ru(NO)(PPh3)]2
    DONG Zhen-Rong, CHENG Da-Dian, WU Zhen-Yi-LI Jian-Lin, ZHAN Meng-Xiong, ZHENG Lan-Sun
    2002, 23(6):  1007-1009. 
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    The fullerene complex, η2-C60[Ru(NO)(PPh3)]2, has been prepared by the reaction of C60 with Ru(NO)(PPh3) under a nitrogen atmosphere and refluxing. The new complex was characterized by means of elemental analysis, IR, XPS, electronic spectra and 31P NMR. The results show that the complex of η2 form can be formed by C60 bonding to Ru(NO)(PPh3)2 in the σ-π way and there is hyperconjugation effect in the molecule. So electrons will flow easier and photoelectric effect for this new compound is expected. In addition, the structure of the complex has been supposed. The ruthenium is 4 coordinate in the complex, bonding to two carbon atoms, to one PPh3 and to one NO.
    Hydrothermal Synthesis and Crystal Structure of a New Polyoxometalate [(CH3CH2)4N]4H3O{Na[(HMo2O5)3(HPO4)(H2PO4)3]2}·(H2PO4)2·10H2O
    ZHANG Hong, XU Lin, WANG En-Bo, HU Chang-Wen, CHEN Jiu-Tong, YAO Yuan-Gen, QIN Ye-Yan
    2002, 23(6):  1010-1012. 
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    The title compound [(CH3CH2)4N] 4H3O{Na[(HMo2O5)3(HPO4)(H2PO4)3]2}·(H2PO4)2·10H2Owas synthesized by hydrothermal method and its structure was determined with single crystal X-ray analysis. The cluster anion of the title compound shows a P1 symmetry sandwich structure. The crystal is triclinic, space group P1 with a=15.1513(2) nm, b=15.8517(10) nm, c=23.0251(10) nm, α-= 89.00(1)°, β-=80.09(3)°, γ = 74.30(2)°, V=5.24190(8) nm3, Z=2, Dc=2.105 g/cm3, F(000)=3270, S =1.039, μ =1. 655 mm-1.
    Preparation of Novel Magnetic Affinity Adsorbents and Application for Purification of Urokinase
    DONG Yu-Sheng, LIANG Feng, JIN Hong-Xia, XI Qi, CHANG Jian-Hua
    2002, 23(6):  1013-1017. 
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    Magnetic dextran microsphere, magnetic agarose microsphere, magnetic polyvinyl alcohol microsphere and magnetic polyhydroxyethyl methacrylate microsphere were activated by epichlorohydrin, N,N′-carbonyldiimidazole or cyanogen bromide on which 6 aminohexanoic acid, glycine, ethylene diamine or 1,6 diamino hexane were bonded as spacers. Then they were coupled with p aminobenzamide, Larginien methyl ester, guanidine hexanoic acid or guanidine acetic acid using N,N′-dicyclohexyl carbodiimide, N-(3-dimethylaminopropyl) N′-ethylcarbodiimide hydrochloride or N,N′-carbonyl diimidazole as coupling reagents. Whereafter 25 magnetic affinity adsorbents were prepared. To test the resolving power of them, magnetic affinity adsorbents were applied to purifying crude urokinase in a batch mode. The effect of some factors such as activators, the length of spacer, coupling reagents and ligands on the rusults of purification was discussed. Good results were obtained. The bioactivity recovery is 40%-70%, the purification fold is between 15 to 40, and the adsorptive capacity varies from 0.08 to 0.2 mg per milliliter adsorbent.
    Synthesis of a Fluorescent Molecularly Imprinted Polymer and Its Recognition Property for Histamine
    DONG He, TONG Ai-Jun, LI Long-Di
    2002, 23(6):  1018-1021. 
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    By using histamine as the template molecule, methacrylic acid as the functional monomer, ethylene glycol dimethacrylate as the crosslinking agent, and zinc(Ⅱ)-protoporphyrin as the functional monomer, a new kind of molecularly imprinted polymer which may emit fluorescence was synthesized. Its binding property was evaluated with a batch adsorption and a column method. The results of both methods indicate that the recognition of histamine with the MIPis superior to that of the NMIP.
    Microgravimetric Amplification and the Detection of Short DNA Sequences on a Quartz Crystal Microbalance by Modified Nano-microspheres
    ZHANG Sheng-Long, PENG Tu-Zhi
    2002, 23(6):  1022-1025. 
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    Anovel and sensitive microgravimetric biosensor has been developed by using actinomycin Dfunctionalized magnetic nano-microspheres, which can be intercalated in duplex strands DNAs on the gold electrode of a quartz crystal microbalance. These modified nano-microspheres have been used as the amplified label for microgravimetric signal owing to their heavy mass. The linear range for the determination of target DNAis from 10-9 to 10-11 mol/L, and the detection limit is found to be 2×10-12mol/L.
    Determination of Activity of Antioxygenation of Glutathione by the "Probe" of the Lactic Acid(LA)-Acetone(Act)-BrO3--Mn2+-H2SO4 Oscillating System
    YANG Shu-Tao, GAN Nan-Qin, LIN Zhi-Xin, CAI Ru-Xiu
    2002, 23(6):  1026-1029. 
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    In our experiment, we applied APPtechnique to study of the perturbation of glutathione(GSH) which is an important antioxidant in vivo on the lactic acid(LA) Acetone(Act) BrO3--Mn2+-H2SO4 oscillating reaction. And we determinate the activity of antioxygenation of GSHby the "probe" of this oscillating system. Influence of experiment variables were investigated, and can be as a base of quantitative analysis. The linear range lies between 1.50×10-7-2.25×10-5mol/L, and the determination limit is 2.20×10-9mol/L. And the precision and throughput were also quite good(1.35% as RSD, and 6-9 samples/h, respctively). Some aspects of the potential mechanism of action GSHon the oscillating systems are discussed.
    The Behavior of Components Transfer in Chip-based Capillary Electrophoresis and Its Characteristics
    WANG Hui, MAO Xiu-Li, GAI Hong-Wei, BAI Ji-Ling, LIN Bing-Cheng
    2002, 23(6):  1030-1034. 
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    On the home made microchip capillary electrophoresis system with laser induced fluorescent(LIF) detection, the electrophoresis behavior of single dye and amino acids labeled with fluorescein 5-isothiocyanate(FITC) was demonstrated on glass chips. The comparison between chip-based electrophoresis and conventional capillary electrophoresis was taken into account. The special attention was paid for the characteristic of chip-based electrophoresis. The effect of various of operation conditions, such as countervoltage, sample loading modes and point of detection, were investigated.
    Modification on the Interface of Capillary Isoelectric Focusing and Mass Spectrometry for Proteomic Research
    XU Chong-Feng, SONG Hao-Wei, YANG Peng-Yuan, WANG Qian, WANG Hong-Hai, XU Yun-Min
    2002, 23(6):  1035-1037. 
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    An important interface modification for capillary isoelectric focusing mass spectrometry(CIEF-MS) is reported. Acapillary needle with a sheath flow tube pre-mounted in one device serves as both the CIEF cathodic-end and the ESI interface. The needle was inserted into the cathode reservoir at the focusing stage, and then removed to the front of sampler orifice of MSat the detection stage. Therefore, the shut-off of the high voltage is not necessary and a better focusing protein zone is maintained during the ESIstage. The optimization of the experimental condition has been investigated and the two dimensional image of the E. coli proteins has been obtained, which is comparable with that from a 2D-gel.
    Ordered Ring Assembly of Cadmium-Calcein Complex Directed Under the Capillary Flow on the Glass Slide Supports and Its Digitalized Fluorescence Image Analysis
    HUANG Cheng-Zhi, LI Yuan-Fang
    2002, 23(6):  1038-1040. 
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    Afluorescent ordered ring assembly was observed under a fluorescence microscope, and the assembly image was captured by using a digital CCDcamera for analytical purposes. When a droplet of diluted solution of cadmium-calcein complex in 0.01 mol/Lhexahydropyridine was spotted onto the surface of dimethyl dichlorosilane modified glass slide, a symmetrical ordered ring was formed with an outer diameter of 1.10 mm and a ring line width of 0.048 mm. It was found that the fluorescent molecules on the ring line followed a Gaussian distribution, and with which a quantitative equation was established. For a 0.1 μLdroplet of the calcium calcein complex, the maximal fluorescence intensity of the ring is proportional to the content of calcium over the range of 3.0×10-15～1.0×10-13mol, and the limit of detection is 2.56×10-16mol. The proposed method has been successfully applied to the quantification of Cd2+ in water samples of Jialingjiang River.
    Chelator Selection in FI-KR-FAAS on-line Preconcentration System
    CHEN Shu-Yu, ZHANG Zhi-Feng, YU Hua-Ming
    2002, 23(6):  1041-1043. 
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    The selection of chelators in the pre concentration system Flow Injection Knotted Reactor Flame Atomic Absorption Spectrometry(FI-KR-FAAS) and their corresponding experimental conditions were studied. Dithione was found to have advantages over the other two chelators with a higher concentration efficiency. Interferences from alkali and alkaline earth elements were overcome; mutual interferences between heavy metals were avoided. Concentration factors of 23.4-69.3 were obtained, with the detection limits of 1.61-2.56 μg/L. The method developed was used to determine certified biological reference materials of human hair, pig liver and sea prawn, and the results agreed well with the certified values, relative standard deviations of the determinations were in the range of 2.10%-3.02%.
    Development of a Piezoelectric Immunosensor for Hepatitis B Surface Antigen
    CHEN Ze-Zhong, WANG Ke-Min, CHEN Yong-Kang, XIAOD an, YANG Xiao-Hai, SHAO Guo-Qiang
    2002, 23(6):  1044-1046. 
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    Apiezoelectric immunosensor has been developed for the detection of Hepatitis Bsurface antigen(HBsAg). Treatment of a Au electrode with cystamine solution results in cysteamine self-assemble monolayers(SAMs). Using a bifunctional cross-linker, glutaraldehyde, the antibody was immobilized on the electrode surface. The influence factors such as the reaction time of immunoreaction and the concentration of antibody etc. were investigated. Under the optimized experimental conditions, a series standard concentration of HBsAg solutions were analyzed in solution. The frequency shift was linear with the antigen mass concentration in the range of 0.2-1.20 μg/mL. The analysis results of two serum specimens showed that the positive serum and the negative serum could be distinguished easily. Glycine HCl solution(0.2 mol/L) was used for desorption of the bound antigen. The crystal could be regenerated nearly 8 times without detectable loss of activity.
    FTIR Study of Microbes
    CI Yun-Xiang, ZANG Kai-Sai, GAO Ti-Yu
    2002, 23(6):  1047-1049. 
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    Distinct spectral differences among Saccharomyces cerevisiae, Corynebacterium glutamicum, Escherichia coli, Staphylococcus aureus were observed from their high quality infrared spectra in the frequence regions 900-1800cm-1 and 2800-3050cm-1. These differences imply that it is possible to use FTIRto analyze and identify microbes. And this method will be a simple, rapid and accurate one.
    Detection of Monoamines in Rat Striatum with Microbore HPLC-ECD
    WANG Lei, HAN Hui-Wan, YU Xiao, ZHAO Rui, LIU Guo-Quan
    2002, 23(6):  1050-1052. 
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    Using microbore HPLCand electrochemical detection, Amicrodialysis HPLCassay system was built. After investigating the linear range, detection limit and reproducibility, this method was used to measure the concentrations of DAand monoamine metabolites in striatal microdialysate with 5 min temporal resolution. The detection limit is less than 5 nmol/L. According to the statistical analysis, the result is stable and accurate. It is very helpful to the physiological, pathological and pharmacological research.
    Applications of Generalized Torsion Angles in Studies on Quantitative Structure-activity Relationship
    ZHANG Qing-You, XU Lu, ZHANG Wen-Jun
    2002, 23(6):  1053-1055. 
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    In this article, generalized torsion angles of derivatives of 1-[(2- hydroxyethoxy)methyl]-6-(phenylthio)thymine(HEPT) were calculated, which include abundant three-dimensional information of molecules. Molecular similarity matrix was built based on the calculated generalized torsion angles. These similarities were taken as the new variables, and the new variables were selected by using Leaps-and-Bounds regression analysis. Multiple regression analysis and neural networks were performed, and the satisfactory results were achieved by using the neural networks.
    Theoretical Study on the Reaction Selectivity of the Catalytic Hydrogenation of 3-Analinomethylidene-5,6-2H-dihydropyran-2,4-diones
    FANG Ya-Yin, SHEN Rong-Xin, SUN Hong-Wei, YUAN Man-Xue, LIU Jie, LI Zheng-Ming, LAI Cheng-Ming
    2002, 23(6):  1056-1059. 
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    Based on diverse groups(R), which located on the 6-substituted site of the dihydropyrandione ring, the final products obtained from the catalytic hydrogenation of 3-analinomethylidene-5,6-2H-dihydropyran-2,4-diones are very different. The selectivity of the title reaction has been studied by means of B3LYP/6-311G**, AM1 semi-empirical method and molecular mechanics (Tripos force field). The results obtained show that the reaction selectivity is decided by the stability of radical intermediate at the first step and the stability is affected by group R.
    Studies on the Asymmetric Total Synthesis of d-Biotin(Ⅴ)
    CHEN Fen-Er, FU Han, MENG Ge, LUO You-Fu, YAN Ming-Guo
    2002, 23(6):  1060-1064. 
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    An efficient, high yielding and stereoselective synthesis of d biotin(6) is described. The stereoselective reduction of the known(3a S, 6a R)-1,3-dibenzyl tetrahydro 4Hthieno imidazol-2,4(1H)-dione(1) with diisobutylaluminum hydride(DIBAL-H) in toluene gave(3a S, 4 S, 6a R)-1,3 dibenzyl-4-hydroxy tetrahydro 1Hthieno imidazol-2(3H)-one(2) in 91% yield with 99.7% e.e.. Alcohol 2 was directly converted into(3a S, 4 S, 6a R) phosphonium salt 3 upon reaction with triphenylphosphine hydrogen tetrafluoroborate. Condensation of the corresponding ylide with 4 formylbutric acid afforded unsaturated acid 4. Catalytic hydrogen transfer hydrogenation of compound 4 with Pd D297 resin/ammonium formate system led stereoselectively to(3a S, 4 S, 6a S)-dibenzylbiotion(5), which was debenzylated by treatment with orthophospaoric acid in the presence of phenol to yield d biotin(6). The overall yield of d biotin was 42% from thiolactone 1.
    Computer Simulation of Human Iodothyronine Deiodinase Single-chain Antibody
    LIN Feng, ZHANG Wei, CHEN Mo, DING Lan, LIU Lan-Ying, XU Xiao-Jie-ZHAOD a-Qing, NI Jia-Zuan
    2002, 23(6):  1065-1068. 
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    Iodothyronine plays a major role in growth, basic metabolism and organ formation. It has an extremely limited source in the body. In this thesis, we designed iodothyronine(T4) as hapten. Then a single chain antibody displayed on phange was obtained from a human phage displaying a single chain antibody library. The specific genes of E3 was subcloned in P-5E vector. According to its amino acid sequences, we simulate its three-dimention structure by computer. It has never been reported in PDB.
    GC-MS Analysis of Ethanol Solution with D2O as Solvent Implanted by Low Energy N+
    SHI Huai-Bin, SHAO Chun-Lin, YU Zeng-Liang
    2002, 23(6):  1069-1072. 
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    Low energy ions were produced by N2 glow-discharge. The positive ones were accelerated into ethanol solution with D2O as solvent to induce chemical reactions. GC-MSanalysis showed that DCH2CH2OH, HOCH2CH2OD were produced by such kind of implantation. Thus, it was proved that the reaction was mainly caused by radicals generated by decomposition of water molecules, D· and ·OD played an important role in the process. Meanwhile, CH3COOD and HOCH2CH2ND2 were also found in the products, so it was concluded that the reaction was carried out under an oxidative atmosphere, which was thought to be probably related to ·OD radicals, too. The capture of Dfrom D2O by N+ to form ·ND2 radicals was not only an initial step to produce HOCH2CH2ND2 but also served as a probable pattern for "nitrogen deposition". All these are helpful to reveal the mechanism of the reaction induced by low energy N+ implanting into solution samples.
    Carbon-13 Enrichment of Rice Stalk Lignin Traced by Solid State 13C NMR Spectroscopy
    GU Rui-Jun, XIE Yi-Min, ZENG Shao-Qiong, WU Hong, Seiichi-Yasuda
    2002, 23(6):  1073-1076. 
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    Carbon-13 enrichment of specific carbon of rice stalk lignin was achieved by feeding coniferin-[ α-13C], coniferin-[ β-13C] and coniferin-[ γ-13C] into an internode cavity of the stalk of a growing rice plant(Oryza sativa L.). The resulting rice stalk tissues were analyzed by high-resolution solid state carbon-13 nuclear magnetic resonance (13C NMR) spectroscopy. It was found that the administration did not affect the normal ligninfication of rice plant. It was also proved that β-O-4, β-β, β-5 and β-1 were mainly a substructure in protolignin of rice stalk although there were some minor substructures as coniferyl alcohol and ferulic acid unit. Importantly, the result indicated that significant bonding occurred at α-position to other constituents, presumed to be mainly of carbohydrates.
    Synthesis, Characterization and Molecular Structure of a Novel Asymmetrical Half-sandwich Binuclear Iron Carborane Complex Cp′2Fe2(CO)3(Se2C2B10H10)
    LU Shi-Xiang, JIN Guo-Xin, HU Ning-Hai
    2002, 23(6):  1077-1080. 
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    The half sandwich methylcyclopentadienyl iron carbonyl complex reacted with 1,2-dilithium diselenolate carborane Li 2Se2C2B10H10 (1) which was produced by the insertion of element Se into 1,2-dilithium carborane to give a half sandwich binuclear iron carborane complex Cp′ 2Fe2(CO)3Se2C2B10H10 (3). X-ray structural analysis of complex 3 reveals that one of the iron atoms is chiral.
    Studies on the Solution Conformations of Bt Toxic CryⅠ Ab Expressed by Bt Transgenic Rice
    WU Zhi-Ping, XU Bu-Jin, SHU Qing-Yao, GONG Li-Qin, YU Hong, YE Gong-Yin, CHEN Zi-Yuan
    2002, 23(6):  1081-1085. 
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    The conformations of the toxic protein CryⅠAb in its solution were studied by fluorescence. The results showed that the toxic protein fluorescence intensity is improved with its pHvalue increase and reaches its maximum at pHequivalent to 11. Adding some organic solvents such as methanol, ethanol, isopropanol result in the emission wavelength of fluorescence of the toxic protein blue shift and its fluorescence intensity increase. However, the toxic protein fluorescence emission wavelength no long blue shifts as these organic solvents concentration beyond certain values. Acetone can quench all fluorescence of the toxic protein CryⅠAb and acrylamide can quench 86% of the total fluorescence of the toxic protein, but KIcan′t quench any fluorescence. It implicates that the most of tryptophan residuals of CryⅠAb are located on the toxic protein surface where the negative charge is rich.
    Separation of Rabbit Liver Metallothionein Sub-isoforms by RP-HPLC with MALDI-TOF-MS Detection
    ZHAO Rui, JI Jian-Guo, YUAN Hong-Sheng, GUAN Hua-Shi, RU Bing-Gen
    2002, 23(6):  1086-1090. 
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    In order to study the sub-isoforms of MTand get their exact primary structure, the mixture and the individuals MT-1 and MT-2 of rabbit liver MTwere separated by different HPLCmethods such as anion exchange and RP-HPLCunder different conditions. The two main MTisoforms MT-1 and MT-2 could be easily isolated from the mixture of MTby anion exchange HPLC. The isoforms of MTs were further isolated by C18 RP-HPLCunder neutral and acidic conditions. All of the isolated isoforms and sub-isoforms were analyzed by MALDI-TOF-MS. The separation of MTisoforms can be obtained by anion exchange chromatography with 50 mmol/L Na2HPO4 NaCl. The sub-isoforms of rabbit liver MTcould be isolated by C18 RP-HPLC. The rabbit liver MT-1 has 3 main sub-isoforms and MT-2 has one sub-isoform. The experiment verified that under different conditions the sub-isoforms of rabbit liver MThas a different apparent molecular mass. This experiment predicted that there would exist a stable peptide structure of MT-2 or its fragment. The primary structure of this peptide component was also studied.
    Size and Shape Recognition of Dye Molecules by Organoselenium-bridged Bis(β-cyclodextrin)s
    CHEN Yong, LI Li, LIU Yu
    2002, 23(6):  1091-1093. 
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    The inclusion complexation behavior of 6,6′-trimethylenediseleno bridged bis(β-cyclodextrin)(1) and 6,6′-(o-phenylenediseleno) bridged bis(β-cyclodextrin)(2) with dye molecules was investigated by means of fluorescence and ultraviolet spectrometric titrations at 25℃ in phosphate buffer solution(pH 7.20). The results obtained indicated that bis(β-cyclodextrin)s could not only significantly enhance the original binding ability of parent β-cyclodextrin, but also be used to recognize the structural difference of guest molecules through the cooperative binding of the closely located two cyclodextrin cavities. This phenomenon was discussed from the viewpoint of size fit concept and multiple recognition mechanism between the host and guest.
    Synthesis of New Multifunctional Chiral C4 Building Blocks from D-Erythorbic Acid
    LI Ming-Xia, WANG Yan-Ming, CHEN Ru-Yu
    2002, 23(6):  1094-1096. 
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    Compounds 4 and 5 which were new selectively protected and multifunctional chiral C4 building blocks were prepared conveniently from commercially available D-erythorbic acid in no more than three steps with satisfied yields. Since compound 4 and compound 5 are densely functionalized and rich in stereochemistry, they are useful chiral building blocks in asymmetric synthesis.
    A Novel Synthesis of Isoxazoles Derivatives
    WANG Jun-Feng, PENG Yun-Gui, DU Bao-Shan
    2002, 23(6):  1097-1099. 
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    The 4-aryl-3,5-bis(methoxycarbonyl)-2-isoxazoline-N-oxides(nitrones)(a) in anhydrous DMFwas refluxed for 3-4 hours and ten of 4-aryl-3,5-bis(methoxycarbonyl)-2-isoxazoles(b) were given with good yields(43%-81%) via thermolysis. All of the 4-arylisoxazoles were identified with IR, 1H NMR, 13C NMR, MS and elemental analysis. Anovel and convenient synthetic method of 4-arylisoxazol was porvided.
    Studies on the Properties of Li-Mn Oxide Made from Various CMD
    ZHAN Hui, ZHOU Yun-Hong
    2002, 23(6):  1100-1104. 
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    Eight typical ways were used to synthesize chemical manganese dioxide(CMD) from which eight types of Li-Mn oxide were prepared. The structures of CMDand Li-Mn oxide were all investigated by XRDexperiment. The results of the electrochemical characterization show that except the structure type, the composition of CMDwhich was used in the preparation can also have a significant influence on the electrochemical performance of the final product—Li-Mn oxide. Even the CMDmaterial was of the same type, the difference under the synthesizing condition could bring out some microcosmic or local change in the structure, which may finally cause the great difference in the electrochemical behavior. Because of its instability at the high temperature, δ-MnO2 was unsuitable to be used as the manganese source for the preparation of the spinel material, although it was characteristic of large tunnel in its structure.
    Synthesis and Characterization of the Composite of Conducting Polyaniline with Fe3O4 Magnetic Nanoparticles
    YANG Qing-Lin, SONG Yan-Lin, WAN Mei-Xiang, JIANG Lei, XU Wen-Guo, LI Qian-Shu
    2002, 23(6):  1105-1109. 
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    Composite of conducting polyaniline(PAn) doped by dodecylbenzenesulfonic acid(DBSA) with Fe3O4 magnetic nanoparticles was synthesized in a neutral solution by a chemical method which was called "modification-re-doped" method. The composite of magnetic nanoparticles modified with doped PAn was synthesized by microemulsion. Then the composite was synthesized by emulsion polymerization extraction method. The composites were characterized by means of FTIR, XRD, UV-Vis, TEM, and SQUID. The results indicate that the composite with superpapramagnetic Fe3O4 nanoparticles possesses a good electrical conductivity and magnetic susceptibility as well as high transmittance.
    Application of 2D Raman Correlation Spectroscopy to Studing the Effect of Rare-earth Eu3+ on Hemoglobin
    XU Jin-Ze, ZHAO Yu, ZHAO Bing, XU Wei-Qing, WU Yu-Qing, LI Zheng-Qiang, ZHAOD a-Qing, XI Shi-Quan
    2002, 23(6):  1110-1112. 
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    The effect of rare earth ion Eu3+ on hemoglobin(Hb) was studied by using two dimensional Raman correlation spectroscopy. The results show that with the variation of Eu3+ concentrations as perturbation, the oxidation state of Hb and its spin state are both sensitive to the perturbation. Eu3+ added to Hb affects the oxidation and spin state synchronously. The four structure sensitive bands of Hb are more accessible to the Eu3+ than other bands.
    Preparation and Structural Characterization of Highly Dispersed γ-Mo2N Supported on Alumina
    MENG Ming, FU Yi-Lu, LIU Zhen-Lin, JIANG Ming, XIE Ya-Ning, HU Tian-Dou
    2002, 23(6):  1113-1116. 
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    The nitrided Mo/Al2O3 catalysts were prepared by temperature programmed reaction between NH3 and MoO3/Al2O3. XRD and EXAFS methods were used for the structural characterization. The results of XRDshow that the molybdenum species in the supported samples exist as a dispersed MoO3 phase before nitriding. After nitriding, most of the molybdenum species were nitrided to form γ-Mo2N. The lower intensity of the radial structure functions of Mo Kedge and the smaller coordination number of Mo-Nshells accordingly indicate that the γ-Mo2Nin the supported samples possesses a high dispersion, the lower the loading of Mo, the higher the dispersion of γ-Mo2Non alumina. From the view of coordination distance, it is found that with the increase of dispersion of γ-Mo2N, the Mo-N distance is a little shortened, which may be resulted from the nano shortening phenomenum. The values of disorder factors show that the γ-Mo2N phase in the supported samples has big thermal and structural disorder extent, and with the increase of its dispersion, both the thermal and structural disorder factors increase.
    Theoretical Studies on the Stabilities of All Possible C40H2 Isomers
    YANG Xia, WANG Gui-Chang, SHANG Zhen-Feng, YANG Zuo-Yin, PAN Yin-Ming, ZHAO Xue-Zhuang
    2002, 23(6):  1117-1121. 
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    The electronic structures of all possible C40H2 isomers and C40 based on D5d symmetry have been calculated with no symmetry constraints at the AM1 and PM3 semiempirical molecular orbital levels. Some rules on addition of H2 to C40 are predicted from the calculations of 51 isomers. Three sorts of main influence factors on isomers stabilities and adding positions, namely, (1) geometric structure of C40, (2) conjugative effect and (3) charge population, are discussed.
    Chiral Recognition Study for the Inclusion Complexes of Amino Acid with β-Cyclodextrin Using a Fast Annealing Evolutionary Algorithm
    XIA Bao-Yun, CAI Wen-Sheng, PAN Zhong-Xiao, SHAO Xue-Guang
    2002, 23(6):  1122-1125. 
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    Chiral recognition of β-amino acid derivatives by charged β-cyclodextrins, mono-NH3+-β-CD, per NH3+-β-CDand per CO2-β-CD, has been studied by using a fast annealing evolutionary algorithm(FAEA) in this paper. The analysis of each energy term shows that the main driving forces of the inclusion complexation are from the electrostatic force and van der Waals forces, and the electrostatic forces are crucial in the enantioselectivity of S/Renantiomers.
    Synthesis, Structure Characterization and Photoactivities of Nanosized Pd Clusters on Titania-modified MCM-41 by Photodeposition Method
    ZHENG Shan, GAO Lian, GUO Jing-Kun
    2002, 23(6):  1126-1130. 
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    Nanosized Pd clusters deposited on titania modified MCM-41 was synthesized by photodeposition method through PdCl42- and titania modified MCM-41. The structure and optical properties of the as synthesized samples were investigated by XPS, N2 adsorption/desorption isotherms, diffuse reflectance UV-Vis absorbance spectroscopy and Raman spectroscopy. Metallic palladium was efficiently photoreduced on the surface of titania in the mesopore from PdCl42- according to the results of XPS. The adsorption revealed that titania and noble Pd clusters were uniformly distributed on the silica wall surfaces of MCM-41 support. The configuration of partial titania in Pd deposited titania modified MCM-41 changed from tetrahedral to octahedral from the results of adsorption in UV-Vis spectra and Raman spectra because of the interactions between the loaded Pd clusters and titania. The Pd deposited titania modified MCM-41 exhibited a high photocatalytic activity for the photodegradation of phenol and the photoreduction of Cr(Ⅵ) to Cr(Ⅲ).
    Reaction Mechanism and Kinetics for the F+ CH2CO Reaction
    HOU Hua, WANG Shao-Kun, WANG Bao-Shan, GU Yue-Shu
    2002, 23(6):  1131-1134. 
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    G3(MP2) theory is used to study the F+CH2COreaction. The calculations reveal a typical addition elimination mechanism for the title reaction. The reaction starts with Fand (CH2CO) reacting with each other to form the activated intermediate (CH2FCO)*. This association reaction is found to be a barrierless process. CH2FCO* can undergo further decomposition and isomerization reactions leading to various possible products. COand CH2Fare found to be the dominant products. RRKM-TST method is used to calculate the total and individual rate constants. The total rate constant shows a weak temperature dependence and a pressure independence.
    Synthesis of MCM-41 in the Presence of CTMABr and CTMAOH
    WAN Ying, WANG Zheng, MA Jian-Xin, ZHANG Yi-Qun
    2002, 23(6):  1135-1139. 
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    Mesoporous molecular sieves MCM-41 with different contents of incorporated structural aluminum were prepared by a modified hydrothermal method using simultaneously two templates. The characterization by using X-ray powder diffraction and nitrogen adsorption techniques revealed that all samples behaved a typical XRDdiffraction of MCM-41, an adsorption isotherm of type Ⅳ and a regular pore size distribution. Although the pore diameter and the uniformity of the pore size distribution were decreased to some extent with the increase of the content of aluminum. The last feature reflects that the Al-MCM-41 prepared by this method has a highly ordered structure of pore arrays. Solid state 27Al MAS NMRinvestigation showed that Al atoms in these samples were incorporated tetrahedrally in the MCM-41 structure, without the existence of extra-framework aluminum. In this paper, the samples prepared by the traditional hydrothermal method were also investigated and compared with those prepared by the new method. The results showed that the purity and formation of cylindrical pore structure of MCM-41 was enhanced by the use of mixed template. The Al atoms could still be incorporated tetrahedrally in the MCM-41 structure even at high level of aluminum. Finally, a theoretical consideration on the simultaneous use of two templates in the synthesis was discussed.
    NOx Adsorption on CeO2-supported ZrO2 Nanometer Powders Prepared in Water-in-Oil Microemulsion
    LI Wei-Bin, YANG Xu-Fei
    2002, 23(6):  1140-1142. 
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    ZrO2 nanometer powders sizing around 5-8 nm were prepared in water in oil(W/O) microemulsion, and TEM, XRD, N2 adsorption were employed to characterize the powders. A Ce-Zr-m sample was obtained after incipiently impregnating the above powders with a Ce(NO3)3 aqueous solution. NOx adsorption was conducted on the sample in a fluidized thermal analysis system and the maximum adsorption amounts of 35.5, 17.5 and 9.5 mg NOx per gram sorbent were obtained at 25, 100 and 200 ℃, respectively, on the Ce-Zr-m sample. It is not worthy that the value at 100 ℃ was 25 times higher than that on the CeO2 supported ZrO2 sample prepared by conventional precipitation.
    The Transition Between the Molecular-ordered Organized Assemblies in the Aqueous Solution of Alkylammonium Chlorides
    LI Yong-Hui, HUANG Jian-Bin, ZHENG Rong, MAO Min, FU Hong-Lan
    2002, 23(6):  1143-1146. 
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    The influences of concentration variation of the aqueous solution of C12 H25 NH3Cl on the molecular-ordered organized assemblies were studied by dynamic light scattering, absorption spectrometry, viscosity and TEM. It is found that the transition process of the micelles vesicles spherical micelles for the morphology of the molecular-ordered organized assemblies took place with the increase of surfactant concentration. Such structure transition can be attributed to the variation of concentration of hydrolytic product C12 H25 NH2.
    Theoretical Study on the Potential Energy Surface of the Reaction of Vinyl Radical (C2H3·) with Hydroxyl Radical(OH·)
    LIU Gui-Xia, DING Yi-Hong, LI Ze-Sheng, HUANG Xu-Ri, SUN Chia-Chung
    2002, 23(6):  1147-1150. 
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    The QCISD(T)/6-311G(2 df,p)//B3LYP/6-311G(d,p) calculations are performed on the mechanism of the radical reaction C2H3·+OH·. Eight products, P1-P8, may be obtained via the complex reaction channels, i.e. association, multi step Hshift, CH3 shift, dissociation, and so on. According to our calculated results, we predict that producets P2 and P6 may be the main products. In this paper, the energy ordering of the transition states TS1/2, TS1′/3 and TS2/3, which connect the C2H4O isomers CH2CHOH(1 or 1′), CH3CHO(2)and CH3COH(3), is TS2/3>TS1′/3>TS1/2, and it is the reverse of the ordering proposed by Wesdemiotis and McLafferty, but in good agreement with Smith et al.′s calculated result.
    Preparation of the Novel Double-functional Composite Electrode and Its Role on the Degradation of Organic Pollutants in Water
    WANG Yu-Ling, CAI Nai-Cai, WANG Ya-Ping, LI Jin, ZHONG Jia-Sheng
    2002, 23(6):  1151-1155. 
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    The methods for preparing the novel composite electrode, the double function of the novel composite electrode and the role of it on increasing the degradation rate of the organic pollutants(such as aniline) in water are introduced. The reaction mechanism is also discussed. The results indicate that when the working potential was controlled at 0.05 Vor so, the composite electrode made up of the carbon PTFE(air) O2 electrode and the TiO2 photo catalyst not only possesses photocurrent effect but also has a high efficiency of generating H2O2. Then the organic molecule in solution can obtain two kinds of roles on degradation coming from the combination of the photo-catalysis and the photochemical oxidation. The rate of degradation of the organic molecule is obviously enhanced.
    Theoretical Study on One-carbon Unit Transfer from5,10-CH+-THF to1,2-Diaminobenzene
    QI Chuan-Song, FENG Da-Cheng, Lü Wen-Cai, KANG Cong-Min, CAI Zheng-Ting
    2002, 23(6):  1156-1159. 
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    Folic acid cofactor plays an important part in different enzymatic one-carbon unit transfer reactions. Its functions have been imitated a lot experimentally by using simple chemical models. One-carbon unit transfer reaction of imidazolinium with 1,2-diaminobenzene has been studied with PM3 semi empirical molecular orbital calculations in this paper. The results show that there are two ways to complete this reaction because the imidazolinium ring has two different breaking patterns. Both of these two ways have six steps, including two proton migrating steps that limit the reaction rate. The structures and energies of the intermediates and transition states have been calculated. All the intermediates and transition states have different conformations, and the reaction of classical conformations has been studied carefully.
    Mechanism of Gas-phase Silylation on Fiber Coating Following Solid Phase Microextraction
    LUAN Tian-Gang, ZHANG Zhan-Xia
    2002, 23(6):  1160-1163. 
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    The silylation of polar analytes on the polymeric coating of SPME fiber could be performed directly by placing the fiber into the headspace of bis(trimethylsilyl)trifluoroacetamide(BSTFA) after SPME . The derivatization was carried out at room temperature without damaging the fiber. Compared with the diazomethane-SPME technique, it is a simpler, cheaper and environmental friendly. The kinetics of the reaction of silylation on SPME fiber coating was studied. The result indicated that the silylation was of pseudo first order kinetics. The reaction depends on the analytes concentration in the fiber coating. The experimental results also show that the new fiber coating has a high extraction efficiency for polar compounds but non-reactive with derivatizing reagents could be found.
    Calculating of Generalized Coupling Coefficients and Matrix Element of Tensor Operators of Chains of Subgroup of SO(4)
    WANG Mei-Shan, DING Shi-Liang, LI Bo-Fu, ZHANG Gang
    2002, 23(6):  1164-1167. 
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    The generalized coupling coefficients of group chains (Ⅰ) and (Ⅲ) were firstly discussed, and then generalized Wigner-Eckart theorem of coupling tensor operators of group chains (Ⅰ) and (Ⅲ) were investigated. We have gained the general expression of reduced matrix element of coupling tensor operators in the third section. As an example, the matrix element of Majorana operator was calculated in the last section. The results shows it is consistent with the result from the literature.
    Ordered Nanostructure of CdS Nanoparticles Assembled by2′-Phosphorothioate Oligo-DNA
    YANG Bai-Quan, JIANG Lin, YANG Wen-Sheng, LI Tie-Jin, LI Pi-Chun
    2002, 23(6):  1168-1170. 
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    CdSnanoparticles were synthesized by using two complementary 2′ phosphorothioate oligo DNA, oligoG 10-SH and oligo C10-SH as stabalizers. Because the thiol group was modified at phosphate site between C1 and C2 of 5′ end, the spatial exposure of DNAresidue at C1 site was preponderant compating with the spatial exposure of the nanoparticles when the DNArenatured. The experimental result showed DNArenaturation ratio is about 50% and CdSnanoparticles were assembled into parallel quadrilateral array as the DNArenaturation progressed.
    Synthesis and Catalytic Performances of Mesoporous Aluminosilicates of Cubic and Hexagonal Structure with Stronger Acid Sites
    LI Gong, KAN Qiu-Bin, WU Tong-Hao, HOU Chang-Min, HUANG Jia-Hui, WU Shu-Jie, LI Can
    2002, 23(6):  1171-1173. 
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    Mesoporous aluminosilicates with cubic and hexagonal structure have been synthesized by structure units of β-zeolite in a two step crystallization process and characterized by XRD, IR, N2 physical adsorption and desorption, 27Al MAS NMRand NH3 TPDtechniques. The results show that MB48(25) and MB41(25) were similar to MCM 48 and MCM-41 on the long range structure respectively and MB48 with a cubic structure can be synthesized under the condition of a lower n (CTMAB)/ n (SiO2) ratio. HMB48(25) and HMB41(25) exhibit a stronger acidic strength than conventional HMCM-41. The catalytic activity of HMB48(25) was the highest for cumene cracking and alkylation of 2,4-tert-butylphenol with tert-butylalcohol.
    Studies on Electrochemical and Catalytic Properties of Poly-m-chloraniline Modified Electrode
    DAI Li-Zong, XU Yi-Ting, ZHOU Shan-Kang, WU Hui-Huang
    2002, 23(6):  1174-1176. 
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    The electrochemical and catalytic properties of PmClAn modified electrode were studied by cyclic voltammetry. The results showed that PmClAn had an excellent electroactivity and proton doping increased the electroactivity. The Pt particles electrodeposited on PmClAn trend towards preferred orientation, and Pt(200) was the preferred face. It was also found that platinized PmClAn promotes isopropanol oxidation, the polymer is not only as a dispersion media of Pt particles forming a "microheterogeneous catalysis system", but also has effect on electronic properties of Pt.
    The Formation of the Reversed Micelle in the Extraction System of Primary Amine N1923
    SONG Xin-Yu, YIN Zhi-Lei, ZHANG Wei-Min, YU Hai-Yun, SUN Si-Xiu
    2002, 23(6):  1177-1179. 
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    The formation of reversed micelle of primary amine N1923 in different solvents is firstly investigated by determining the interfacial tension and electric conductivity in the organic phase and the IRspectra. Asignificant difference has been discovered for the formation of reversed micelle between the sulfate and the chloride.
    Studies on Photochemical Oxidation of Nitrophenols in Seawater
    YANG Gui-Peng, QI Jia-Lin
    2002, 23(6):  1180-1182. 
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    The photochemical degradation of p-nitrophenol and 2,4-dinitrophenol in both natural seawater and artificial seawater was studied under the irradiation of mixed light sources(ultraviolet lamp/high pressure mercury lamp). The photolysis of the two nitrophenols was influenced by various factors including medium, heavy metal ions and photosensitizer. The photolysis of the two nitrophenols in natural seawater was faster than in artificial seawater, presumably due to the effect of inherent photosensitizers in natural seawater. The addition of Cu2+, Pb2+ or Cd2+ into the seawater solutions obviously increased the photolysis rate of the nitrophenols. Interestingly, we found that the presence of anthroquinone could accelerate the photolysis of p-nitrophenol in natural seawater but had almost no impact on the photolysis of 2,4-dinitrophenol. The half-lives of the photoreactions in natural seawater under our conditions were 40-54 min for p-nitrophenol and 37-69 min for 2,4-dinitrophenol, respectively. Our study suggests that photochemical degradation is an important removal pathway for the nitrophenols in seawater.
    Non-isothermal Crystallization Behavior and Kinetics of Metallocene Short Chain Branched Polyethylene
    PENG Ya, FU Qiang, LIU Jie-Ping, HE Tian-Bai
    2002, 23(6):  1183-1188. 
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    The non isothermal crystallization behavior and kinetics of metallocene short chain branched polyethylene were investigated via DSCat cooling rates from 2.5 to 20 ℃/min, and subsequent heating at rate of 10 ℃/min. To verify the effect of molecular weight and branching content on crystallization, three group samples were chosen: (1) linear polyethylene with low molecular weight and high molecular weight; (2) low molecular weight polyethylene with low branching content and high branching content; (3) high molecular weight polyethylene with low branching content and high branching content. The results show that crystallization temperature, crystallinity, melting temperature and crystallization rate are highly branching content dependent. Molecular weight effect is less important, compared to branching content. Adramatic decrease of crystallization temperature, crystallinity, crystallization rate and melting temperature was observed for branched samples. The non isothermal kinetics was analyzed via the methods developed by Gupta and Mo Zhi shen, and good agreement was obtained.
    Relationships Between Structures and Hydrolytic Stability of Silazane Compounds
    JIANG Jian, PENG Wen-Qing, ZHENG Zhi-Min, XU Cai-Hong, XIE Ze-Min
    2002, 23(6):  1189-1192. 
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    Relationships between structures of a series of silazane compounds and their hydrolytic stability were investigated by contacting silazane compounds directly with water vapor. It was indicated that steric hindrance of substituents strongly influenced hydrolytic stability of silazane compounds. Compounds with bigger substituents had better hydrolytic stability. As for cyclosilazanes, hydrolytic stability was also dependent on ring strength. However, steric hindrance played more dominant roles. Cyclosilazanes with phenyl substituents, hexaphenylcyclotrisilazane and polymeric compounds containing Si-N bond were of excellent hydrolytic stability due to high steric hindrance.
    Studies of Mocrotribological Property on the Self-assembly Films from Diazoresin and C60-containing Polyelectrolyte
    HUANG Lan, GU Qian-Yi, HE Yuan-Kang, LUO Guo-Bin, ZHAO Xin-Sheng, CAO Wei-Xiao
    2002, 23(6):  1193-1197. 
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    The star-shaped C60-styrene-acrylic acid copolymer [C60-poly(S-AA)] was synthesized successfully. The layer-by-layer self-assembly diazoresin/C60-poly(S-AA) films were fabricated. The crosslinking structure formed from the conversion of ionic bond to covalent bond after UVirradiation. The roughness and microtribological property of these C60-containing films were investigated by AFM/FFM, which shown the films are promising for lubrication materials.
    In-situ UV-Vis Spectra of Polyaniline Doped with Protonic Acid in Organic Solvent and Its Resolution with Factor Analysis
    YANG Chun-Ming, CHEN Di-Zhao, FANG Zheng, LIU Ye-Xiang
    2002, 23(6):  1198-1201. 
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    In situ UV-Vis spectra for protonic acid doping reaction of polyaniline in organic solvent were recorded. The doping reaction mechanism was obtained from the chemical factor analysis for the first time. The results show that two competing reactions might exist during the doping process: one is the dynamic equilibrium between doping and dedoping reaction, and the equilibrium constant being k = 5.16(24 ℃); the other is a side reaction. The product of the side reaction should be a doped mixture between intrinsical and doped states formed during the reaction.
    Self-assembly and Photovoltaic Property of Covalent-attached Multiplayer Films Based on Poly[(4-carboxyphenyl)acetylene] and Diazoresin
    YAO Gui-Jun, DONG Yu-Ping, CAO Ting-Bing, YANG Shu-Ming, Jacky-Wing-Yip-Lam, TANG Ben-Zhong
    2002, 23(6):  1202-1204. 
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    Anovel multiplayer film was assembled from poly[(4-carboxyphenyl)acetylene](PCPA) and diazoresin(DR) in aqueous solution via electrostatic attraction. Under UVirradiation, following the decomposition of diazonium group between the adjacent interfaces of the multiplayers, the ionic bonds of the self-assembly film convert to covalent bonds and the film becomes very stable toward electrolyte solutions. Thus the photoelectric conversion property of poly[(4-carboxyphenyl)acetylene] containing film can be measured in conventional three-electrode photoelectrochemical cell, and 0.5 mol/L KCl solution can be used as the supporting electrolyte. The photocurrent spectroscopy responses coincide with the absorption spectrum of the irradiated self-assembly film, which indicates that the irradiated DR/PCPAfilm is responsible for the photocurrent generation.
    Fabrication of Three-dimensional Microstructure by Argon Ion Laser Curing of Epoxy Resin
    ZENG Zhao-Hua, WANG Xia, YANG Jian-Wen, WANG He-Zhou, CHEN Yong-Lie
    2002, 23(6):  1205-1206. 
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    Visible light curable photoresist consisting of epoxy resin Epon SU8 and iron arene photo initiator Irgacure 261 was used to fabricate three-dimensional microstructure by means of three-dimensional holographic lithography technique. Argon ion laser with wavelength of 488 nm was used as light source in the experiments. Field emission microscope diagram showed the formation of three-dimensional microstructure. It was found that the amount of photo-initiator, the laser intensity and the exposure time are the key factors to obtain well defined three-dimensional microstructure.
    Studies on the Phase Behavior of Ternary Random Copolymer Blends
    LI Guang-Xian, TANG Ping
    2002, 23(6):  1207-1209. 
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    A spinodal equation based on the modified Prigogine-Flory′s equation of state theory was derived and applied to predicting the phase behavior of a ternary polymer blend comprising styrene-methyl methacrylate copolymer(SMMA),styrene-acrylonitrile copolymer(SAN)and poly methyl methacrylate(PMMA). According to Flory′s combining rules, the parameters of state equation for copolymers were evaluated from those of the constituent monomer segments, and binary segmental contact energy parameters Xij between copolymer and copolymer were computed. The numerical solution of spinodals of SMMA-PMMA-SAN at various temperatures was derived by computer programming, and confirmed by the corresponding experimental results. It was found that Flory′s equation of state theory could be successfully extended to predict the phase behavior of ternary copolymer blends by adding the term of interaction entropy parameters Qij evaluated from the phase diagrams of the corresponding binary blends.
    Immobilization of Gelatin onto Polyurethane Membrane Surface and Acceleration of Endothelial Cells Growth
    GAO Chang-You, YUAN Jun, GUAN Jian-Jun, SHEN Jia-Cong
    2002, 23(6):  1210-1212. 
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    Gelatin was covalently immobilized onto the polyurethane membrane surface grafted previously with poly(methacrylic acid) (PU-g-PMAA) using 1-[(3-dimethylamino)propyl]-3-ethyl carbodiimide as the condensing reagent. ATR-FTIR and ESCAcharacterizations verify the occurrence of the grafting, and prove that the immobilized amount of gelatin is proportional to the number of active sites, i.e. carboxylic groups on PU surface. Endothelial cells culture reveals that the cell attachment and cell growth on PU-g-PMAA-g-Gelatin are both improved obviously, demonstrating that a cell compatible PUis obtained and the immobilizing method is quite effective to introduce cell growth factors onto polymer surface.
    Fabrication of Self-assembly Ultra-thin Film Based on Sulfonated Polyaniline and Diazoresin and Its Photoelectric Conversion Property
    CAO Ting-Bing, YANG Shu-Ming, ZHANG Mao-Feng, HUANG Chun-Hui, CAO Wei-Xiao
    2002, 23(6):  1213-1215. 
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    Through self-assembly technique, a new type of layer-by-layer ultra-thin film was fabricated based on water-soluble substituted polyaniline and photosensitive diazoresin through electrostatic attraction. Under UVirradiation, the bond nature between layers turns from ionic to covalent following the decomposition of diazonium group, and the film gets very stable. The photoelectric conversion property of substituted polyaniline containing self-assembled film has also been investigated in this article.
    Topography of Polyhydroxybutyrate Banded Spherulites
    XU Jun, GUO Bao-Hua, ZHANG Zeng-Min, CHEN Guo-Qiang, WANG Xiu-Feng
    2002, 23(6):  1216-1218. 
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    On polyhydroxybutyrate banded spherulites, concentric rings were observed between cross polarizers or without polarizers. The rings used to be considered as cracks. In this paper, we provide evidences to distinguish the concentric rings from cracks observed on PHBspherulites. Furthermore, atomic force microscopy confirmed that these concentric rings with varying spacing were growth terraces rather than cracks. The height of the terraces reached up to several hundred nanometers. It was observed that the external terraces were higher than the internal terraces, which was proposed to result from layer-by-layer growth. This is the first report on the new microscopic feature of polyhydroxybutyrate spherulites. Spherulites with birefringent bands, wavy fluctuation of height were also observed.
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