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    10 August 2006, Volume 27 Issue 8
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    高等学校化学学报2006年第27卷第8期目次
    2006, 27(8):  0.  doi:
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    研究论文
    Synthesis of Mesoporous Silica at Room Temperature and Near-neutral pH with EDTANa2 as Mineralization Agent
    XIAO Qiang1, WANG Jin-Gui1, GAO Di1, SUN Ping-Chuan1, YUAN Zhong-Yong1, CHEN Tie-Hong1, LI Bao-Hui2, DING Da-Tong2
    2006, 27(8):  1395-1399.  doi:
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    Using EDTANa2 as mineralization agent, mesoporous silicas with wormlike mesopores and thick pore wall(about 3 nm) were facilely synthesized at room temperature and near-neutral pH. The mesoporous silica can be obtained with reactants molar composition range of n(CTAB):n(TEOS):n(EDTANa2):n(H2O)=(0.05—0.2):(0.1—2):(0.1—0.5):(100—500). XRD, N2 sorption, FTIR, SEM and TEM methods were carried out to investigate the topological and morphological properties of the mesoporous silicas. As the amount of CTAB increased, the d spacing value of mesoporous silica increased correspondingly. Temperature has a great effect on the synthesis of mesoporous silica. When temperature increased from 2 ℃ to 20 ℃, morphologies of the mesoporous silica varied from hollow micro-tubes to granule aggregates. Based on the experiments, a modified neutral mechanism of (S+-E-)0-I0 was proposed.
    Synthesis, Characterization and Crystal Structure of a New Layered Heterometallic Coordination Polymer {[(CuL)2Sr(H2O)·Sr2(H2O)7]·2H2O·0.5CH3OH}n
    TAO Ruo-Jie1, LIU Bao-Lin1, LI Fu-An1, CHENG Yan-Xiang2, NIU Jing-Yang1
    2006, 27(8):  1400-1403.  doi:
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    A copper-strontium heterometallic coordination polymer was synthesized and characterized by elemental analysis and IR spectra. The crystal structure was determined by single-crystal X-ray diffraction analyses. The title complex is a 2D coordination polymer with the chemical formula {[(CuL)2Sr(H2O)·Sr2(H2O)7]·2H2O·0.5CH3OH}n, where H4L=N-(2-hydroxybenzamido)-N'-(3-carboxylsalicylidene)ethylenediamine. Its structural unit is comprised of two adjacent units, which polymerized with each other to form a new layered heterometallic coordination polymer.
    Surface Chemical Modification of Onion-like Fullerenes
    XU Bing-She1, SUN Rui-Ping1, HAN Pei-De1, LI Tian-Bao1, WANG Xiao-Min1, LIU Xu-Guang2
    2006, 27(8):  1404-1408.  doi:
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    Onion-like fullerenes(OLFs) synthesized by chemical vapor deposition(CVD) were purified by dilute nitric acid. The microstructures of OLFs and purification effects were analyzed by TEM and TGA respectively. Then OLFs were refluxed with potassium in toluene and were characterized by using FTIR and Raman spectroscopy. It is found that the wavenumbers at 3451, 1402 and 1039 cm-1 show characteristic peaks of hydroxyl groups indicating the formation of OLFs(OH)n. The raman results reveal, the ratio of IG/ID increases, graphitization degree of OLFs is improved and the D line and G line of OLFs have no obvious changes before and after reaction, which indicate that OLFs retain their structures.

    研究论文
    Synthesis and Crystal Structure of a Novel Superamolecular Compound Based on Imidazole Functionalized Sandwich Type of Tungstobismutate
    LIU Hong1,2, XU Lin1, QIU Yun-Feng1, AN Wen-Jia1, JIN Ya-Na1, XU Bing-Bing1
    2006, 27(8):  1409-1412.  doi:
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    A novel superamolecular compound, Na8H[{Na(H2O)}3{Mn(C3H4N2)}3(BiW9O33)2]·32H2O, was synthesized under the open-air conditions, and characterized by X-ray single-crystal diffraction, IR spectra and elemental analysis. The crystal belongs to hexagonal system, space group P6(3)/m with a=1.394 8(4) nm, b=1.394 8(4) nm, c=3.348 6(19) nm, γ=120°, V = 5.641(4) nm3, Z=12. The crystal structure consists of two α-B-BiW9 subunits and displays a sandwich type polyanion linked by three Mn2+ ions between the two α-B-BiW9 units and the Mn2+ ions coordinate an imidazole molecule, respectively. Thus, this compound can be considered as a new kind of inorganic-organic hybrid materials. Moreover, three neighboring [[{Na(H2O)}3{Mn(C3H4N2)}3(BiW9O33)2]9- polyanions form a triangle cavity through the nonclassical hydrogen bonds and such units extend further along ab plane to construct two-dimensional layered framework. Such two-dimensional layered structure further pack each other interlacedly along c axis to construct an interesting three-dimensional supramolecular framework containing a one-dimensional hexagonal channels.
    Studies on Luminescence Properties of Lanthanide Complexes Based on Pyrazolone
    SHEN Li1, SHI Mei1, SHI En-Xian2, DU Yu-Kou2, LI Fu-You1, HUANG Chun-Hui1
    2006, 27(8):  1413-1417.  doi:
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    A series of lanthanide(Tb3+, Eu3+, Sm3+, Dy3+, Gd3+) complexes with 1,3-diphenyl-4-phenyl-acetyl-5-pyrazolone were synthesized and characterized by elementary analysis, FTIR and UV-Vis spectra. The Eu3+ complex was further characterized by X-ray diffraction. The luminance properties of the lanthanide complexes were studied in detail. Importantly, the triplet energy level of the ligand was measured with reference to the phosphorescence spectrum of its gadolinium complex, and the difference between the ligand's triplet energy level and the excited energy level of lanthanide ion results in different photoluminescences of the corresponding complex.
    研究简报
    Synthesis and Crystal Structure of a 3D Metal-organic Framework Microporous Compound Cd5(BTC)4(H2O)8·6H2O
    SUN Fu-Xing1, ZHU Guang-Shan1, YE Ling2, FANG Qian-Rong1, QIU Shi-Lun1
    2006, 27(8):  1418-1420.  doi:
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    The title compound, Cd5(BTC)4(H2O)8·6H2O(BTC=1,3,5-benzenetricarboxylate) was synthesized under mild conditions, and its crystal structure was determined by means of single crystal X-ray diffraction. The compound crystallizes in the monoclinic system and belongs to space group P21/c with a=1.0226(2) nm, b=1.0814(2) nm, c=2.9876(6) nm, β=99.437(3) °, V=3.2591(11) nm3, Z=2, Dc=1.645 g/cm3, Mr=807.23, μ=1.691 mm-1, F(000)=1544, GOF=1.082, R=0.0592, wR=0.1877. Its structure revealed that Cd1 and Cd2 centers are firstly linked with BTC to form wave-like layers, and then the octahedral coordination geometries of Cd3 centers connect the neighboring above layers to construct the 3D framework of Cd5(BTC)4(H2O)8·6H2O having “Z”-like shaped channels with the greatest dimensions about 2.6 nm viewed along the [100] direction.
    In-situ Synthesis and Activity of Nano-hydroxyapatite/Lysozyme Composite
    WANG Chun-Yan1,2, ZHU Guang-Shan1, GAO Bo3, WANG Run-Wei1, LI Juan2, XIN Ming-Hong1, QIU Shi-Lun1
    2006, 27(8):  1421-1423.  doi:
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    Nano-composite of hydroxyapatite/lysozyme with a size of 100 nm was synthesized in situ by chemical wet method, and characterized by nitrongen gas adsorption method, IR, SEM and UV-Vis spectroscopic techniques. In comparison with that synthesized by the dipping adsorbing method, the composite synthesized by wet method has much more content and activity of lysozyme. These results suggest the composite can be used as a controlling carrier of releasing lysozyme.
    研究论文
    Measurement of Oil-Water Partition Coefficients by Improved Microemulsion Electrokinetic Chromatography
    JIANG Xue-Mei1,2, WEI Wei-Li1, JIANG Jun-Po1, SHI Kai-Yun2, MU Xiao-Jing1, CHEN Zhi-Tao2, XIA Zhi-Ning1,2
    2006, 27(8):  1424-1429.  doi:
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    Microemulsion electrokinetic chromatography(MEEKC) was used as a powerful method for the indirect measurement of oil-water partition coefficients of organic compounds. Considering the problems of determining oil-water partition coefficients by conventional MEEKC, the concentration of solute and high electric-field having impact on the migration behavior of compound was studied, the reason and mechanism of which were also studied. Moreover, an improved method of MEEKC(I-MEEKC) that can be used to solve the problems found was developed. Applying this improved method to determining oil-water partition coefficients for compounds, such as alkyl-benzene: benzene, toluene and ethyl benzene, good result was obtained: the average error between oil-water partition coefficients estimated by using improved MEEKC and literature values published was 0.07 logarithm units. In this work not only a new method was established to measure oil-water partition coefficients with MEEKC, but also the improved MEEKC is developed further and become more reliable and more accurate method for qualitative analysis.
    Studies on Phenylethanoid Glycosides in Plant Extract of Plantago asiatical by Electrospray Ionization Multi-stage Tandem Mass Spectrometry
    LI Li1,2, LIU Zhi-Qiang1, LIU Chun-Ming2, TSAO Rong3, LÜ Lei1, LIU Shu-Ying1
    2006, 27(8):  1430-1434.  doi:
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    The structures of phenylethanoid glycosides in plant extract from Plantago asiatica were successfully analyzed and identified by electrospray ionization multi\|stage tandem mass spectrometry(ESI-MSn) in the negative ion mode, the fragmentation mechanisms of phenylethanoid glycosides were explored according to some interesting losses. The rapid identification of the phenylethanoid glycosides in plant extract of Plantago asiatica was developed.
    Studies on a Chemiluminescent Immunoassay with the Erythrocyte-labeled Antibody
    ZHANG Wen-Yan1,2, WEI Jing-Yan1, GUO Jie3, CHEN Gui-Qiu4, XING Cheng3, SHI Li-Hua5, YUAN Wei2, QIAN Li-Na2, QUE Xiao-Dong2, GAO Li2, LIU Meng-Hong2
    2006, 27(8):  1435-1438.  doi:
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    A novel chemiluminescence immunoassay suitable for the determination of the hepatitis B virus' surface antigen(HBsAg) was studied. Instead of the enzyme-labeled antibody in enzyme-lined immunosorbent assay(ELISA), the erythrocyte-labeled monoclonal anti-HBsAg antibodies were utilized as the second antibody in this double antibody sandwich immunoassay. After the sandwich immunoreaction occurs, the sensitized erythrocyte, having combined with the immune complex made from antigen and the first antibody, suffers from hemolysis in low osmotic solution and releases hemoglobin(Hb). Hb can catalyze the chemiluminescent reaction of luminal by hydrogen peroxide. The intensity of the chemiluminescent reaction was linearly with the concentration of the hepatitis B virus' surface antigen(HBsAg) in the detected samples. This assay can be used to detect 0.5 ng/mL of HBsAg. The 30 healthy donors and 30 patients with hepatitis B were detected for HBsAg with this method and with routine ELISA as the standard. The coincidence rate of the two assays was 97%, which illustrates that the developed chemiluminescence immunoassay with erythrocyte-labeled antibody is suitable in clinical determination.
    Desorption Electrospray Ionization Mass Spectrometry for Direct Analysis of Clinic Urine Samples
    CHEN Huan-Wen1, LI Ming1, ZHOU Jian-Guang1, FEI Qiang1, JIANG Jie1, JIN Qin-Han1, ZHANG Tian-Mu2, ZHANG Xie3
    2006, 27(8):  1439-1442.  doi:
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    DESI-MS was applied to direct simultaneous detection of multiple components of clinic urine samples without any sample pretreatment. Under the optimized working conditions, such as ESI infusion rate, ESI high voltage, incident angle, collective angle, tube lens voltage, etc., for both DESI and LTQ mass spectro-meter, the main components of urine including urea, pyruvic acid, creatinine, oxalic acid, alloxane, menadione were detected as the protonated molecules in positive detection mode using methanol-water(volume ratio 1:1) as the spray solvent in the low mass range(15—200 amu). Sodium and potassium were also detected but mainly in the form of clusters with urea and creatinine. In each case, the corresponding ions were isolated in the ion trap mass analyzer and underwent a collision-induced dissociation process, which yielded characteristic fragments in tandem mass spectra and resulted in confident validation of the analytical results. The average time for single sample analysis was less than 1 min since it required no sample pretreatment. Furthermore, the semi-quantitative analysis of the components was also demonstrated by adding serine as an internal standard into the samples.
    Preparation and Properties of Dibutyltin Molecularly Imprinted Polymer
    SUN Xiang-Ying, ZHOU Zheng, LIU Bin
    2006, 27(8):  1443-1447.  doi:
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    By using dibutyltin(DBT) as the template molecule, chitosan as the functional monomer and glutaraldehyde as the cross-linking monomer, dibutyltin molecularly imprinted polymers(DBT-MIPs) were synthesized by the molecular imprinting technology. In this paper, the structure of DBT-MIPs was characterized with scanning electronic microscope, and the synthesis conditions of DBT-MIPs, the adsorption properties and selective recognition of DBT-MIPs for DBT were also studied. The experimental results show that DBT-MIPs has a high adsorption capacity and good selective recognition for DBT, and the maximum adsorption capacity of DBT-MIPs is 178.6 μg/g.
    Comparative Investigation on Acute Biological Effect of Lanthanum and Cerium by MAS 1H NMR-based Metabonomic Approach
    LIAO Pei-Qiu, WU Hui-Feng, ZHANG Xiao-Yu, LI Xiao-Jing, LI Zhong-Feng, LI Wei-Sheng, WU Yi-Jie, PEI Feng-Kui
    2006, 27(8):  1448-1452.  doi:
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    High-resolution magic-angle-spinning(MAS) 1H NMR spectroscopic and pattern recognition(PR) based methods were applied to compare the different acute biochemical effects between La(NO3)3- and Ce(NO3)3-treated rats. Male Wistar rats were treated with various doses(2, 10, 50 mg/kg body weight) of La(NO3)3 and Ce(NO3)3, and MAS 1H NMR spectra of the intact liver and kidney tissues were analyzed by using principal components analysis to extract metabolic information. The target lesion of La(NO3)3 to liver and Ce(NO3)3 to both liver and kidney were found by MAS 1H NMR-PR methods. This work illustrated that the combination of NMR and pattern recognition technique is a powerful method to study the biochemical effects induced by xenobiotics.
    研究简报
    Determination of Escherichia Coli. O157:H7 in Food Based on Chemiluminescent Magnetic Enzyme-linked Immunoassay
    ZHU Guang-Hua1, HE Yan-Feng1, GUO Xiao-Ying2, LIU He-Ping3
    2006, 27(8):  1453-1455.  doi:
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    A high sensitive chemiluminescent magnetic enzyme-linked immunoassay method was established for Escherichia coli. O157:H7 determination. The bacterium antibody was labeled by alkaline phosphatase(ALP) that catalyzed the decomposing of substrate 3-(2-spiroadamantane)-4-methoxy-4(3-phosphoryloxy)phenyl-1,2-dioxetane(AMPPD) to give the light emission. The sensitivity of the method is 8.5×104 Cell/mL with a linear range of 1.0×105—5.0×107 Cell/mL. The intra- and inter-assay CVs are 14.8% and 20.0% in pork samples, respectively. The correlation coefficient of present and the standard plate counting method is 0.981. The experiments with the spiked samples show that this method has great potential to be applied to detecting the concentration of Escherichia coli. O157:H7 in a variety of samples.
    An Improved PMP Derivatization Method for Analyzing Monosaccharide Composition
    LIN Xue1, WANG Zhong-Fu1, HUANG Lin-Juan2, BAI Quan1, JIA Jing-Fen1
    2006, 27(8):  1456-1458.  doi:
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    An improved carbohydrate derivatization method employing 1-phenyl-3-methyl-5-pyrazolone(PMP) was developed in this study. Liquid ammonia was used instead of sodium hydroxide aqueous solution to provide the base medium for the derivatization reaction. Derivatization reaction and HPLC separation conditions were optimized, including reaction time, reaction temperature and PMP consumption. The derivatives of five reducing monosaccharides were well separated by HPLC. Because we employed ammonia instead of sodium hydro-xide, the excessive volatile ammonia can be removed by vacumm drying, these derivatives could be directly analyzed by MALDI-TOF-MS without desalting procedure, possessing potential application for monosaccharide and oligosaccharide separation and subsequent MS analysis. This method not only increased the MS detection sensitivity, but also decreased sample wastes during purification. We successfully applied this method to mo-nosaccharide composition analysis of polysaccharides SPPA-1, SPPB-1 and SPPC-1 purified from Spirulina Platensis.
    Determination of Mitoxantrone via Ammonium Molybdate Using High Sensitive Resonance Rayleigh Scattering Method
    WANG Fen, LIU Zhong-Fang, LIU Shao-Pu, HU Xiao-Li
    2006, 27(8):  1459-1461.  doi:
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    In 0.12 mol/L hydrochloric acid and nitric acid media, mitoxantrone interacted with molybdate to form an ion-association complex, which can result in the significant enhancement of RRS intensity. The maximum scattering wavelengths were 365 nm for RRS and scattering intensities are proportional to the concentration of mitoxantrone, which can be applied to the determination of mitoxantrone. The detection limits are 6 ng/mL in nitric acid and 8 ng/mL in hydrochloric acid respectively. Because there are not such interactions between anthracycline anticancer drugs such as daunorubicin and epirubicin with molybdate, mitoxantrone can be determined selectively with other anthracycline anticancer drugs existing. The optimum experiment condition, affecting factor and the effect of coexisting substance were investigated in the paper. The application to the determination of mitoxantrone in serum and urine by RRS were not only sensitive but also simple and ra-pid. In addition, the interaction mechanism was discussed.
    研究论文
    Analysis and Comparison of Serum Proteomics of Senescence Accelerated Mice
    JIANG Ning1, ZHOU Wen-Xia1, ZHANG Yong-Xiang1, ZHANG Xue-Min2, WANG Jie2, LIU Bing-Yu2
    2006, 27(8):  1462-1466.  doi:
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    To analyze and compare differential serum proteins of senescence accelerated mice: SAM-prone/8(SAMP 8) and SAM-resistance/1(SAMR 1), the proteins of sera from 6 and 12 month-old SAMP 8 and age-matched SAMR 1 were separated, detected and analyzed. Compared with the same age SAMR 1, 15 proteins expressions in sera of six-month-old SAMP 8 were up-regulated, 3 proteins expressions down-regulated significantly and 7 proteins only expressed in SAMP 8 sera; 9 proteins expressions in sera of twelve-month-old SAMP 8 were up-regulated, 7 proteins expressions down-regulated significantly and 12 proteins only expressed in SAMP 8 sera. Using MALDI-TOF-MS, 19 proteins with significant changes were identified by peptide fingerprinting-map and the results searched in MASCOT database. The results showed that 6 proteins were only expressed in sera of six-month-old SAMP 8, 4 proteins only expressed in sera of twelve-month-old SAMP 8. In addition, there were 9 common proteins presenting both in sera of six and twelve-month-old SAMP 8. Our study showed that there were significant differences in serum protein expressions between SAMP 8 and SAMR 1, and some differential proteins may result in pathological changes during the course of aging.
    Different Protein Expression of Myocardium from Chinese Mini-swine Model of Myocardial Infarct
    ZHAO Yan-Feng, YE Neng-Sheng, ZHANG Rong-Li, FENG Xue, LUO Guo-An, WANG Yi-Ming
    2006, 27(8):  1467-1471.  doi:
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    High-resolution two-dimensional polyacrylamide gel electrophoresis(2DE), followed by computer assisted image analysis was used to screen protein patterns of normal and infarcted cardiac muscle tissue for quantitative and qualitative differences in protein expression. In the gels of pH=5—8 IPG strips, 851 protein spots were detected in normal cardiac muscle tissues and 1 032 protein spots were resolved in infarcted cardiac muscle tissues. Thirteen protein spots were only expressed in normal cardiac muscle tissues, and 14 protein spots were only expressed in infarcted cardiac muscle tissues. The results also showed that 49 protein spots displayed quantitative changes in expression between normal and infarcted cardiac muscle tissue. Eleven protein spots were subjected to MS analysis and 7 proteins were identified by PMF. These proteins may be involved in the cardiovascular injury, and play an important role for the future treatment of coronary heart disease.
    Synthesis of 5-[1-Aryl-pyrrol-2-yl]-1H-tetrazole
    LIU Wei1, MA Yuan1, YIN Ying-Wu2, ZHAO Yu-Fen1
    2006, 27(8):  1472-1475.  doi:
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    In this paper, tetrazole ring systems were sythesized by using readily available materials via anodic cyanations of suitably N-substituted pyrrole as key step. The electrooxidation of several 1-arylpyrroles was carried out in methanol containing sodium cyanide at a Pt anode in a divided cell. In all instances, replacement of a heteroaromatic hydrogen by a cyano group occurred regio-selectively. The corresponding pyrrole cyanides were obtained in yields ranging from 76% to 85%. The advantages of electrochemistry synthesis of pyrrole cyanides are as follows: the reaction condition is simple, the cost is low and the products is highly pure. The new tetrazole derivatives which may be non-peptidic compounds with potential angiotensin Ⅱ antagonist properties, were synthesized by the formal [2+3] cycloaddition of NaN3 and pyrrole cyanides.
    Syntheses of Novel Organogermanium Compounds Containing α-Amino Acid and Studies on the Antitumor Activity
    CHEN Jian-Xin1, CHEN Li1, ZHAI Yu-Ping2, SHI Yin2, SUN Li-Juan1
    2006, 27(8):  1476-1479.  doi:
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    In order to search new organogermanium antitumor drugs with an activity and low toxicity, 20 new organogermanium compounds were designed and synthesized by attaching α-amino acid to organogermanium moieties. Their structures were confirmed by IR, 1H NMR and elemental analysis. The crystal structure of Ph3GeCH(Ph)CH2CONHCH(CH2COOC2H5)COOC2H5 were determined by X-ray diffraction. Three human neoplastic cell lines(KB, HCT-8 and Bel-7402) were used to screen these compounds. The results indicate that some compounds at 5 μmol/L show a weak in vitro antitumor activity.
    研究简报
    A New Norneolignan from Cephalomappa Sinensis
    MEI Wen-Li1,2, DAI Hao-Fu1, WU Da-Gang2
    2006, 27(8):  1480-1481.  doi:
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    Cephalomappa sinensis(Euphorbiaceae) is a monotypic genus ever-green tree endemic to the calcareous mountainous region in southwest of Guangxi Zhuang Autonomous Region. Its fresh branches are used as feeding stuff for cattle, horse, sheep, and can make them strong. To find the possibility of developing feed additive or medicine for livestock, the chemical constituents from this plant were studied. The chemical constituents of its roots had been reported in our earlier papers. In continuation of our investigation on the branches of Cephalomappa sinensis, a new norneolignan, named Ceplignan(1), was isolated from ethanol extract through column chromatography. The structure was elucidated on the basis of spectroscopic evidence.
    Isolation and Structure Characterization of a New T-Superfamily Conotoxin from Conus Caracteristicus
    LIU Shang-Yi, CAO Ying, ZHAO Ting-You, DAI Xian-Dong, ZHONG Ming-Nai, FAN Chong-Xu, CHEN Ji-Sheng
    2006, 27(8):  1482-1484.  doi:
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    Cone snails are tropical marine predatory molluscs, and there is an unprecedented variety of neuropharmacologically active peptide. Over seventy living species of cone snails are distributed in China. The ve-nom of Conus caracteristicus collected from South China Sea was studied in this work. A new conotoxin, cr5a, was isolated from the venom through Sephadex G-25 chromatography and HPLC, and then was identified by amino acid analysis, mass spectrometry, N-terminal sequence. The primary structure of cr5a was CCKFQFLNFCCNE, it shared a conserved T-superfamily of conotoxins arrangement of cysteine residues(CC-CC). Total chemical synthesis of the two possible disulfide linkages of cr5a was achieved, and the result of HPLC co-elution showed that cr5a was a tridecapeptide with a disulfide connectivity of Cys1-Cys10, Cys2-Cys11. So cr5a is a new member of the T-superfamily conotoxins.
    Separation, Purification and Structural Identification of the Phytotoxin from Nimbya Alternantherae
    ZHOU Yi-Pin1, XIANG Mei-Mei1, JIANG Zi-De2, LI Hua-Ping2, SUN Wei1, LIN Hai-Lin1, FAN Huai-Zhong2
    2006, 27(8):  1485-1487.  doi:
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    Nimbya alternantherae is a leaf spot fungus isolated from Alternanthera philoxeroides. It could produce phytotoxin to Alternanthera philoxeroides in several kinds of liquid media, especially in modified Fries. The filtrate of the pathogen was chromatographed on a DM-130 colophony column eluting with methanol, and evaporation of the solvent gave a brown mush. The crude product was then extracted with ethyl acetate. The toxin could be purified as white needles by re-crystallizing from benzene and acetone(volume ratio is 1:1) and silica gel chromatograph. The results of elemental analysis, MS, IR and NMR indicate that molecular weight of the toxin was 240, formula was C11H12O6, and its chemical name was 2-acetyl-3,4-dihydroxy-5-methoxyphenyl-acetic acid(Vulculic acid ).
    研究论文
    Synthesis of TiN Nanocrystals with High Specific Surface Area by Hydrazide Sol-gel Method
    LIU Mei-Ying, YOU Wan-Sheng, LEI Zhi-Bin, ZONG Xu, YING Pin-Liang, LI Can
    2006, 27(8):  1488-1491.  doi:
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    Nanocrystalline TiN with a high specific surface area was successfully prepared by the hydrazide sol-gel method with N2H4 as the nitrogen source. The effects of Ti sources, heat-treatment atmospheres, and temperature on the crystallization of TiN powder were studied and the crystallization mechanism of TiN nanocrystals was also discussed. TiCl3 is superior to TiCl4 and isopropoxide in the formation of well-crystallized TiN nanocrystals. NH3 has the advantage over N2 and Ar in the complete removal of residual carbon in TiN powder. In comparison with the traditional temperature-programmed reduction under flowing NH3 atmosphere, the hydrazide sol-gel route requires a relatively low temperature on the one hand(600 ℃) and TiN powder prepared by this synthetic approach exhibits a small particle size(10 nm) and an exceedingly high specific surface area(>135 m2/g) and disperses uniformly on the other hand. We expect that this methodology will provide a novel low-temperature route to synthesize nanocrystalline transition metal nitrides through choosing hydrazine as N-source precursor.
    Influences of Zn on Active State of Sn in Pt-Sn/γ-Al2O3 Catalysts and Propane Dehydrogenation
    YU Chang-Lin1,2, XU Heng-Yong1, GE Qing-Jie1, LI Wen-Zhao1
    2006, 27(8):  1492-1495.  doi:
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    The effect of Zn addition to Pt-Sn/γ-Al2O3 catalyst on the activity and selectivity in the reaction of propane dehydrogenation was studied. The results show that the addition of Zn to Pt-Sn/γ-Al2O3 catalyst can greatly improve the performance of Pt-Sn/γ-Al2O3 for propane dehydrogenation. The initial conversion of propane increased from 34% to 42% and initial selectivity to propene increased from 80% to 98%. At the same time, the presence of Zn greatly reduced the deactivation rate. The studies of temperature-programmed reduction of hydrogen(H2-TPR) and temperature-programmed electronic conductivity(TPEC) show that the addition of Zn to Pt-Sn/γ-Al2O3 made the reduction of Sn become more difficult. This may suggest that the presence of Zn can stabilize tin promoter in an active oxidation state and prevent the formation of PtSn alloy in strong reduction atmosphere, which may be responsible for the high stability and selectivity for Pt-Zn-Sn/γ-Al2O3 catalyst in dehydrogenation.
    A Theoretical Study on Reaction Between Fluorinated Acetyl Peroxy Radical[CF3C(O)O2] and HO2 Radical
    ZHOU Yu-Zhi1,2, ZHANG Shao-Wen1, LI Qian-Shu1
    2006, 27(8):  1496-1499.  doi:
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    A DFT study on the reaction mechanism between CF3C(O)O2 and HO2 radicals was carried out. It is suggested that both the triplet and singlet potential surfaces involve a complex mechanism. The reaction prefers to occur on the singlet surface to produce fluorinated acetic acid and ozone.
    Preparation of Nanostructured Cobalt Thin Film Electrode and Its Abnormal Infrared Effects
    CHEN Qing-Song, LI Jun-Tao, ZHOU Zhi-You, YAN Jia-Wei, SUN Shi-Gang
    2006, 27(8):  1500-1504.  doi:
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    Nanostructured thin film of cobalt supported on glassy carbon (nm-Co/GC) was prepared by electrochemical deposition under cyclic voltammetric conditions. SEM studies illustrated that the Co film was composed of most irregularly small Co nanoparticles with an average size of 150 nm and a few large Co particles of diameter ranging from 400 nm to 500 nm. In situ FTIR spectroscopy employing CO adsorption as the probe reaction revealed that the nanostructured Co film exhibited abnormal infrared effects. The unique anomalous IR features of CO adsorbed on nm-Co/GC consist of the inversion of the COad IR bands, the significant enhancement of IR absorption of COad, and the large Stark effect as well as broadening of the COad IR bands (the FWHM of COL on nm-Co/GC is 8 cm-1 larger than that on bulk Co). The current investigation can extend the study of AIREs to nanomaterials of metals of iron family, and gain an insight into the origin of particular properties of nanomaterials.

    Simulation Calculation of Structure and IR Spectra of Alkyllimidazolium Chloroaluminates Molten Salts
    WANG Peng1, WANG Da-Xi1, GAO Jin-Sen1, DONG Kun1,2, XU Chun-Ming1, LIU Jing-Jiang3
    2006, 27(8):  1505-1508.  doi:
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    Geometry and IR spectra data of (EMIM)AlCl4, (PMIM)AlCl4, (BMIM)AlCl4 and (EMIM)Al2Cl7 were calculated successfully by the density function theory(DFT). Compared with the experimental data, the computational results are identical to them and credible. The unknown geometry and IR data of the compounds were predicted and the ionic liquids[(BMIM)AlCl4 and (BMIM)Al2Cl7] were synthesized and their structures were determined by IR spectra. The geometry and IR data simulated by quantum chemistry were demonstrated.
    Delamination and Aromatic Amine Intercalation of LayeredMicroporous Aluminophosphate
    WANG Chen, PENG Li-Ping, HUA Wei-Ming, YUE Ying-Hong, GAO Zi
    2006, 27(8):  1509-1512.  doi:
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    The delamination and intercalation of layered microporous aluminophosphates [Al3P4O16]•[CH3CH2NH3]3 and [Al2P3O10(OH)2][C6NH8] with aromatic amine were carried out and followed by XRD and SEM measurements. The basicity of amine plays an important role in this process besides the dielectric constant of the solution and the amount of amine added. A saturated benzylamine(pKa=9.34) intercalates of the aluminophosphate are obtained while no aniline(pKa=4.60) intercalates are formed under the similar conditions. The remarkable effect of basicity of the amine can be explained by a metathetical balanced reaction model. The influence of layer structure on the delamination and intercalation processes is discussed as well.
    Studies on Hydrothermal Synthesis of Titania with Different Morphologies and Degradation of Phenol
    SHI Jin-E, YAN Ji-Chang, WANG Yue-Hong, YAN Fu-Cheng, CHEN Da-Wei, WANG Ying, ZHAO Kai, LI Xiao-Kun, CUI Xiao-Ying, ZHAI Yu-Juan
    2006, 27(8):  1513-1517.  doi:
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    Different crystal and crystalline type titania nanoparticles were prepared by using the hydrothermal method and controlling the pH values of solution, ratios of the reactants, temperature and time of hydrothermal reaction. The experimental results show clearly that uniform rod-like titania particles in an average aspect ratio of 4:1 could be obtained under the condition of the pH=11, n(TBOT):n(TEA)=1:2, hydrothermal treatment at 150 ℃ for 48 h. When the pH of the solution was less than 10, spherical titania nanoparticles could be obtained; but when the time was changed to 24 h, spindle titania particles could be obtained. The nanoparticles prepared above are all anatase, but when the pH more than 12, the particles turn to brookite. Phenol in polluted water was used as the degeneration model and the photocatalytical activity of titania with different morphologies was tested in this article.
    Preparation and Surface Enhanced Raman Spectroscopic Studies on Au-Ag Alloy Nanoparticles
    WANG Mei, YAO Jian-Lin, GU Ren-Ao
    2006, 27(8):  1518-1521.  doi:
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    Au-Ag alloy nanoparticles with different molar ratios were prepared by using sodium citrate as the reducer, and the size was increased via the NH2OH\5HCl-growth method. One plasmon band between that of monometallic Ag and Au observed in their UV-Vis spectra indicated the formation of Au-Ag alloy nanoparticles. TEM results showed diameters about 60 nm and homogeneous color of the alloy nanoparticles without clear core-shell contrast. By using thiophenol as the probe molecules, SERS studies were performed. The results indicated the SERS effect was dependent on the composition and size of the alloy nanoparticles. At the certain sizes of nanoparticles, the SERS intensities were increased gradually with the increase of gold content except Au25Ag75. As Au25Ag75 were smaller than Ag, the size effect made the SERS intensity of Au25Ag75 lower. While aggregating way of Au50Ag50 and Au75Ag25 after adding TP molecules were gradually close to Au, and the surface plasma resonance of aggregates approached to 1064 nm, so SERS of TP at higher Au content was controlled by surface plasma resonance enhancement of aggregates.
    A New Route to Direct Synthesis Styrene Carbonate from Styrene Catalyzed by Quaternary Ammonium Bromide
    SUN Jian-Min1, WANG Ya-Li1, QU Xue-Jian1, JIANG Da-Zhen1, XIAO Feng-Shou1, Fujita Shin-ichiro2, Arai Masahiko2
    2006, 27(8):  1522-1525.  doi:
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    This paper reports a novel and convenient synthetic route to styrene carbonate from styrene and CO2 catalyzed by quaternary ammonium(phosphonium) salts, which avoids the isolation of intermediate epo-xide. This route involves two sequential reactions: epoxidation of styrene and cycloaddition of CO2 to epoxide. With tetrabutylammonium bromide as the catalyst, oxidants have a strong effect on the carbonate yield. The influences of reaction temperature, reaction time, CO2 pressure and catalyst amount are studied in detail. Under mild reaction conditions(80 ℃, 6 h, CO2 pressure 1 MPa), the yield of styrene carbonate can be increased to 38% with TBAB without any organic solvent. Moreover, the synergistic effect of bulky ammonium cation and moderate nucleophilicity of anion results in its good performance in the one-pot synthesis of styrene carbonate.
    Separation of DFT Energy and the Study on π-ElectronDelocalization Energy in Benzylideneaniline
    MA Yan-Ping, BAO Peng, YU Zhong-Heng
    2006, 27(8):  1526-1529.  doi:
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    Köster's method for separating the DFT energy of benzene into π and σ parts is used to investigate the nature of the π delocalization energy in a nonplanar molecule benzylideneaniline(NBA). Contrary to the classical viewpoints, the vertical resonance energy ΔEV is always destabilizing, and it is most destabilizing at about θ=0° geometry at B3LYP/6-31G*, 6-311G*, 6-31G(2d), 6-311G(2d) levels. Besides, the one electron energy of the π system is more sensitive to π delocalization than that of the σ system. Furthermore, it is the electronic coupling between the π and σ electrons, rather than the π-π and σ-σ interaction, that plays a main role in determining Coulomb and the exchange-correlation energy effects associated with the π interaction between fragments.
    Molecular Simulation for the Chemical Equilibrium of Methane Steam Reforming in Slit Pores
    PENG Xuan, WANG Wen-Chuan
    2006, 27(8):  1530-1534.  doi:
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    Reactive Canonical Monte Carlo (RCMC) simulation was performed to investigate the chemical equilibrium of methane steam reforming in slit pores. In this simulation, CH4, CO and H2 are all described as spherical Lennard-Jones molecules, the potentials of H2O and CO2 are calculated by TIP4P and EMP2 models respectively, and the Steele's 10-4-3 model is used to represent the interaction between a Lennard-Jones site and the solid wall. Because of no experiments reported for the reaction in slit pores, the chemical equilibrium compositions in bulk phase from RCMC method are compared with those from classic thermodynamic prediction. The good agreement from both methods indicates that it is reasonable to predict the chemical compositions in the pore phase from RCMC simulation. Finally, the effects of other factors on the chemical equilibrium are predicted.
    Quantum Chemistry Research in Etherification of Isoamylene and Methanol
    SHEN Yong-Li, CAO Ying-Yu, YANG En-cui, HAO Jin-Ku
    2006, 27(8):  1535-1539.  doi:
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    The mechanism of the reaction of 2-methyl-1-butene and 2-methyl-2-butene with methanol to yield TAME was theoretically studied by ab-initio H-F/6-31G*. The results show that the reaction includes two elementary reactions. First, isoamylene reacts with proton to produce tert-carbonium intermediate, then the intermediate reacts with methanol to produce the final product TAME. The activation energy of the resulting tert-carbonium from 2-methyl-1-butene and 2-methyl-2-butene are E1=2.26 kJ/mol, E2=7.72 kJ/mol respectively. The activation energy of the resulting TAME from methanol and tert-carbonium is E3=1.29 kJ/mol, so the formation of tert-carbonium is the rate-determining step, and the rate of etherification of 2-methyl-1-butene is quicker. For both 2-methyl-1-butene and 2-methyl-2-butene translate into tert-carbonium intermediate under the acidic condition, and the intermediate need to overcome E'1=4.40 kJ/mol, E'2=63.11 kJ/mol when it translate into 2-methyl-1-butene and 2-methyl-2-butene again, so it is very hard for it to translate into alkenes again. The isomerization of different alkenes didn't exist in this reaction.
    Investigation of Microstructure-machining on Aluminium Surface by Confined Etchant Layer Technique
    JIANG Li-Min1, 2, HUANG Xuan-Min2, TIAN Zhong-Qun1, TIAN Zhao-Wu1
    2006, 27(8):  1540-1544.  doi:
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    This work aims to develop confined etchant layer technique (CELT) to fabricate three-dimensional (3D) microstructures of aluminum substrate for microelectromechanical systems (MEMS). In spite of the fact that LIGA technique is current method for metal bulk micromachining with a high aspect ratio, it is extremely difficult to be applied to aluminum because the electrodeposition as one of the process for LIGA is not suitable for using molten salt at a high temperature. The important feature of CELT is to use a scavenger in solution to efficiently consume the etchant so as to confine the etchant as an ultrathin layer on the working electrode surface (mold electrode). The outer boundary of the diffusion layer of the etchant can retain the three-dimensional fine micro-pattern of the mold electrode. The key issue to successful fabrication of microstructures with CELT is the design of an appropriate “generating-scavenging” system for etchant. In the present study, NaNO2 was electrochemically oxidized into HNO3 so as to etch the aluminum workpiece. The thickness of H+ diffusion layer was confined by reacting with NaOH as the scavenger. The etched pattern of aluminum was observed to be approximately the negative copy of the mold with the precision of 504 nm. The chemical and electrochemical processes were analyzed. The influences of processing parameters, such as current density and scavenger concentration, were discussed. Our preliminary result demonstrates that CELT has a potential to be developed as an effective technique for micromachining 3D microstructures of aluminum, which can be applied for fabrication of micro electromechanical systems.
    Study on Interfacial Adsorption Behavior of Bovine Serum Albumin on Air-water Interface and Its Interaction with Chiral Probes D/L-N-[4-(1-Pyrene)butyroyl]-phenylalanine
    ZHAI Chun-Xi, MA Li-Jun, LI Li-Na, WU Yu-Qing, LI Wen, WU Li-Xin
    2006, 27(8):  1545-1548.  doi:
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    Surface pressure vs. time(π-t) curve was applied to studing the interfacial adsorption behavior of bovine serum albumin(BSA) and the chiral discrimination of it to D/L-N-[4-(1-pyrene)butyroyl] phenylalanine(PPs) on the air/water interface. The conformational changes of BSA induced by the interactions with PPs were also investigated. The results suggest that stable monolayer of BS underwent a slow progress of conformational rearrangement. It is apparent that the specific interactions between PPs and BSA depend both on the concentration and the isomeric specificity of the probes. At a high concentration, PLP and PDP inhibit the surface activity of BSA strongly. However, at a certain low concentration, they work oppositely. And compared with PLP, PDP can bind more effectively with BSA on the air/water interface.
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    Volumetric Properties of Amino Acids in Aqueous D-Xylose Solutions at 298.15 K
    XU Li1, WANG Xu1, MA Lin2, LIN Rui-Sen1
    2006, 27(8):  1549-1551.  doi:
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    Densities of glycine, L-alanine and L-serine in various aqueous D-xylose solutions were measured at 298.15 K by an Anton Paar Model 55 densimeter. Apparent molar volumes, limiting partial molar volumes and hydration numbers for these amino acids were calculated. The transfer volumes from water to aqueous D-xylose solutions were obtained and discussed in terms of the structural hydration interaction model. The results show that all of the transfer volumes are positive, and increase with increasing xylose concentration; the side-chain contributions to the transfer volumes are highly related to the nature of side-chain groups; the hydration numbers for the three amino acids in solutions decrease with increasing xylose concentration.
    In Situ ATR-FTIR Study on the Interaction of HA with Bovine Serum Albumin
    YE Qing, HU Ren, LIN Zhong-Yu, LIN Chang-Jian
    2006, 27(8):  1552-1554.  doi:
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    In situ ATR-FTIR was used to study the interaction of bovine serum albumin(BSA) and hydroxyapatite(HA) in this work. Both on the electrochemically deposited HA and self assemblied titanate nanotubes(TNT) substrates, the adsorption of BSA increases with the increase of time, and its adsorption on HA surface is much larger than that on TNT surface, implying that HA has a good biocompatibility as a biomaterial. It is indicated that Ca2+ plays an essential role in the protein absorption on the HA surface, due to that BSA is negatively charged, and it is able to combine with cation locations in HA particles by electrostatic forces. It is found that, when reacting with BSA, the phosphate band of HA in solution shifts to higher wavenumbers, indicating that PO43- can also be an adsorption site for BSA. The spectroscopic study on the interaction between HA and BSA will be helpful for further understanding the nano hydroxyapatite bioproperties on molecular level.
    Preparation of Nanocrystalline ZnO on the Surface of Kaolinite by Microwave Heating and Mechanism Analyses for Its Formation
    ZHANG Xian-Ru, GU Xiao-Wen, SUN Jia, XU Zheng
    2006, 27(8):  1555-1557.  doi:
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    ZnO nano-powders was prepared on the surface of exfoliated kaolinite(with the precursor solution of ZnAc2·2H2O and ammonia) via microwave heating hydrolysis method, the nanocrystalline ZnO was characterized by using XRD, FTIR, TEM and their formation mechanism was proposed. The results indicate that the products are composed of hexagonal-phased ZnO. The morphology of ZnO is rod-like without exfoliated kaolinite(length is 100—200 nm, diameter is 50—80 nm) as well as is cluster whisker-like in the presence of exfoliated kaolinite(length is 200—350 nm, diameter is 40—60 nm). The infrared absorption of the latter was enhanced apparently. The formation mechanism of the nanocrystalline ZnO synthesized by this method was also suggested.
    Studies on Initial Kinetics of Room-temperature Solid-solid Reaction by UV-visible Reflection Spectrum
    TANG Xin-Cun1,2, HUANG Bai-Yun2, HE Yue-Hui2
    2006, 27(8):  1558-1560.  doi:
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    In this paper, the method of UV-visible reflection spectrum(UV method) was theoretically and experimentally proposed to investigate the initial kinetic characters of the solid-solid reaction with the mixture of dimethylglyoxime and Ni(Ac)2·4H2O, and the mixture of dimethylglyoxime and anhydrous Ni(Ac)2 as the modeling reaction examples. The results indicated that the UV method was very sensitive in the initial period of solid-solid reaction. The reactive rates for above two reaction systems were varied non-linearly with the change of reaction time. The fastest reaction rates can be reasonably explained by the formation of the cold-melting layer or cold-dissolving-melting layer.
    研究论文
    Coordination Polymerization of n-Octyl Isocyanate Catalyzed by Rare Earth Phosphonate/Alkylaluminium System
    YANG Xiong-Fa, NI Xu-Feng, SHEN Zhi-Quan
    2006, 27(8):  1561-1565.  doi:
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    Coordination polymerization of n-octyl isocyanate catalyzed by rare earth phosphonate catalyst Nd(P204)3 using Al(i-Bu)3 as cocatalyst was carried out at -10 ℃ to obtain poly(n-octyl isocyanate) with a high molecular weight and narrow molecular weight distribution. Under the optimal polymerization conditions: n(Al)/n(Nd)=10 aging at 50 ℃ for 5 h, n(n-OctNCO)/n(Nd)=100, polymerized at -10 ℃ for 10 h in bulk, producing a polymer with 88.3% yield, Mn=38.9×104, and MWD=3.53. The kinetics and mechanism of the polymerization were investigated.
    Recognition Performance of o-Phthalic Acid-Cu(Ac)2 Molecular Imprinting Polymers
    WANG Jun, LÜ Tian, ZHAO Mei-Ping, LI Yuan-Zong
    2006, 27(8):  1566-1569.  doi:
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    Molecularly imprinted polymer(MIP) was synthesized by using the complex of o-phthalic acid-Cu(Ac)2 as the template. The experimental results show that Cu(Ac)2-o-PA imprinted polymer[P(PA/Cu)] has selective binding to its template complex, including selectivities to the anions, cations and o-PA analogues of the complex. The possible structure of the complex Cu(Ac)2-o-PA is also proposed according to the crystal structures of similar systems. According to the results, the acetate in Cu(Ac)2 also participated the imprinting process and is a part of the template. Therefore, it plays an important role in the recognition of template and its analogue complexes. Additionally, the high retention of o-PA-imprinted polymer[P(PA)] toward Cu(Ac)2-o-PA and similar Cu-complexes over o-PA itself is well explained by the binding similarity between 4-VP/o-PA and 4-VP/Cu(Ac)2-o-PA. The metal ion-mediated imprinting approach of present study may find applications for the compound which can not be directly imprinted.
    AFM Studies on UV-initiated Grafting of Glycidyl Methacrylate onto High-density Polyethylene Surface
    WANG Hui-Liang
    2006, 27(8):  1570-1574.  doi:
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    The microstructure of grafted polymer chains has a significant effect on the final properties of the grafted polymer, however, there is still not a direct method to characterize the microstructure of grafted chains. The microstructure of the grafted chains formed in the initial stage of the UV-initiated photografting of glycidyl methacrylate(GMA) onto high-density polyethylene(HDPE) surface and the initiation rate of the surface photografting reaction were studied with tapping mode atomic force microscopy(AFM). The grafted materials with granular structures were found on HDPE surface after 30 s UV irradiation, after that, the number and the volume of the granules increased with the increase of irradiation time. The granule was thought to be a single grafted chain with a highly branched(or superbranched) microstructure. The grafting density on HDPE increased almost linearly with the increase of irradiation time in the range of 30—45 s, and the increasing rate of grafting density became slower after 45 s. The initiation rate of surface photografting was about 6.5 Unit/(μm2·s) in the range of 30—45 s.
    Synthesis of Amphiphilic Diblock Copolymer Poly(10-hydroxydecanoic acid)/poly(glycidyl methacrylate) by Combining Enzymatic Condensation Polymerization and ATRP
    LI Dong-Shuang1, SHA Ke1, LI Ya-Peng1, LIU Xiao-Tian1, AI Peng1, WANG Wei1, CHEN Liang2, WANG Jing-Yuan1
    2006, 27(8):  1575-1578.  doi:
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    The diblock copolymers poly(10-hydroxydecanoic acid)-block poly(glycidyl methacrylate)(PHDA-b-PGMA) were synthesized by combining enzymatic condensation polymerization of 10-hydroxydecanoic acid(HDA) and atom transfer radical polymerization(ATRP) of glycidyl methacrylate(GMA). PHDA was firstly obtained via enzymatic condensation polymerization catalyzed by Novozyme-435. Subsequently one end of PHDA chains was modified by reaction with α-bromopropionyl bromide and the other was protected by chlorotrimethylsilane(TMSCL), respectively, the resulting monofunctional macroinitiator was used in the ATRP of GMA using CuCl/2,2'-bipyridine(bpy) as the catalyst system to afford the diblock copolymers including biodegradable PHDA blocks and well-defined PGMA blocks. Polymer nanospheres were prepared by the self-assembly behaviors of the amphiphilic diblock copolymers PHDA-b-PGMA in aqueous solvent.
    Preparation and Properties of Composite Film of Poly(imidesiloxane) Copolymer/Polyimide with Different Performances on Each Side
    YANG Jing-Jing, ZHOU Hong-Wei, DANG Guo-Dong, CHEN Chun-Hai
    2006, 27(8):  1579-1582.  doi:
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    In order to make normal PI films with some new characteristics to be used as microelectronic materials, such as excellent adhesive properties and low electric constants, a novel kind of PI composite film containing different contents on each surface was prepared with chemical surface-modification, from poly(imidesiloxane) copolymer and polyimide. First, poly(imidesiloxane) copolymer was synthesized from 4,4'-oxydianiline(ODA), α,ω-aminopropylpoly(dimethylsiloxane)(PDMS) and 3,3',4,4'-biphenyltetracarboxylic dianhydride(s-BPDA). Then, a THF solution of the copolyamide acid and a DMAc solution of the polyamide acid were mixed thoroughly and doctored on a glass plate dried at RT, and then with thermal imidization to get the composite film. All characterization results from X-ray photoelectron spectroscopy(XPS) and contact angle measurements show that the PDMS has segregated to the air surface and predominated in it. Moreover, the composite film has nearly the same excellent thermal properties and mechanical properties as the normal PI films.
    Investigation of Short Range Ordering in Amorphous PES Copolymer by Means of Radial Distribution Functions Derived from X-ray Diffraction
    ZHOU Xiao-Ming, GAO Zhong-Min, LI Xiang-Shan, JIANG Zhen-Hua
    2006, 27(8):  1583-1586.  doi:
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    The short range order(0—1.5 nm) in polyether sulfone(PES) copolymer samples were studied. The result showed that two intra-molecular distances in the copolymer repeat unit were successfully resolved in the RDF pattern. However, there were only a suggestions of broad peaks at r≈0.55 nm and r≈1.1 nm attributable to intermolecular ordering, indicating that little intermolecular ordering occurred in either sample. The appearance of the two peaks at ~0.5 nm period suggested the existence of more or less parallel chain segments in PES copolymers. A annealed sample was examined to assess the sensitivity of the RDF method to short range intermolecular ordering. The RDF plot of this annealed sample showed a small variety compared with the quenched PES copolymer sample. The RDF parameter showed that the short range order in PES copolymer samples was essentially affected by the annealing procedures. The results of electron-microscopy investigation of PES copolymer sample, heat-treated at 200 ℃ for 72 h, indicate that the copolymer molecular aggregation is changed from a randomly coiled amorphous phase to an ordered one.
    研究简报
    Supramolecular Hydrogel Formed from Gelator with Low Molecular Weight Based on Hydrogen Bonds
    WANG Yu-Jiang, TANG Li-Ming, WANG Yan
    2006, 27(8):  1587-1589.  doi:
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    A building unit(defined as SBU) synthesized from 1,2,4,5-benzene tetracarboxylic acid and 4-hydroxy pyridine was used as the gelator with low molecular weight to form supramolecular hydrogels at various concentrations. The dried hydrogels(xerogels) were observed by scanning electron microscope(SEM). The results indicate that the xerogels possess network structures composing of intertwined fibers and the dimension of the fibers can be regulated by the concentration of SBU. Powder X-ray diffraction(XRD) analysis indicates that the fibers are connected by SBU building units. The reversible sol-gel transition of the supramolecular system with the change of temperature was also noticed.
    Study on PTC Behavior of Modified CF-EVA Composite Materials
    WANG Ke1,2, ZHANG Guo1,2, LI Zhuo-Shi1,2, LIU Xiu-Qi1,2
    2006, 27(8):  1590-1592.  doi:
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    Carbon fiber oxidized by KMnO4 was combined with ethylene vinyl acetate(EVA) copolymer, the obtained composite shows a fine stability of thermal cycles and nearly unchanged switching temperature under thermal cycles, at the same time negative temperature coefficient(NTC) phenomenon is eliminated. Solvent-extraction method is used to examine the interaction between EVA and CF and insolublity with the gel structure were found. The crosslinking network in the gel adsorb CF intensely which makes CF disperse in EVA uniformly, orientate consistently, combine with EVA tightly and shows the elimination of NTC phenomenon. The switching temperature of the composite in the heating process is not identical with that of the composite in the cooling process absolutely, but the temperatures in the above two processes are consistent with the outset of melting temperature and the end of crystallization temperature respectively.
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