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Table of Content

    24 August 2001, Volume 22 Issue 8
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    Articles
    Encapsulation and Catalytic Activity of Lipophilic Soluble Metallophthalocyanine Derivative in MCM-41
    BAI Ni, ZHANG Ping, GUO Yang-Hong, PANG Wen-Qin, SONG XI-Ming, CHEN Hong-Mei, LI Biao, CHANG Xiao-Hong
    2001, 22(8):  1275-1278. 
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    Lipophilic soluble metallophthalocyanine derivative Co(Ⅱ)-4,4',4″,4"-tetrapropy-loxycarbonyl phthalocyanines CoPc[COO(C3H7)4)4] has been encapsulateDInto MCM-41 by impregnation wetness method, then the composites were characterized by XRD, UV-Vis diffuse reflectance spectra, TGA-DTA, Raman spectrum and N2 adsorption methods. At last, their catalytic properties on the oxidation of 2-mercaptoethanol have been examined. Compared to bulk metallophthalocyanine molecule, excellent catalytic properties have been shown for the composite.
    Sol-gel Synthesis and Properties of Ce1-xGdxO2-x/2 Solid Solutions
    JIANG Kai, PENG Cheng, LI Wu-Ju, WANG Lin-WANG Hong-Yan, LIANG Hong-Wei, MENG Jian
    2001, 22(8):  1279-1282. 
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    Aseries of solid electrolytes Ce1-x Gdx O2-x/2 ( x=0-0.6) was prepared by sol-gelmethod. The structure, thermal expansion coefficient and electrical properties of the solid solutions were systematically studied. XRDdata showed that a complete cubic fluorite structure was formed at 160 ℃. The purity of the product prepared by the sol gel methoDIs higher, the grain size is uniformly smaller. They were easily sintereDInto highly dense ceramic pellets at 1300 ℃. The sintering temperature was significantly lower than that by traditionally high temperature solid phase reaction method. The thermal expansion coefficient of Ce0.8 Gd0.2 O1.9 , determined from high-temperature XRDdata, is 8.125×10-6 K-1 . Impedance spectra analyses showed that the grain boundary resistance of the solid electrolyte prepared by sol-gel method was reduced or even eliminated. The conductivity of Ce0.8 Gd0.2 O1.9 is 5.26×10-3 S/cm at 600 ℃. The activation energy ( Ea) is 0.82 eV.
    A Study of PrGa1-xMgxO3 as the Electrolytes of SOFCs
    LIU Zhi-Guo, HUANG Xi-Qiang, LIU Wei, Lü Zhe-JI, Yuan-PEI Li, HE Tian-Min, SU Wen-Hui
    2001, 22(8):  1283-1285. 
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    PrGa1-x Mgx O3( x=0, 0.05, 0.10, 0.15, 0.20, 0.25) were synthesized by using a standard solid state technology. XRDresults show that all samples are orthorhombic. Mg-doping increases the oxygen ion conductivity and decreases the activation energy of the samples significantly. The conductivity of the samples is mainly ionic. PrGa0.9 Mg0.1 O3 has the highest conductivity of 0.05 S/cm at 800 ℃, while PrGa0.8 Mg0.2 O3 has the lowest activation energy of 24.19 kJ/moLIn all the samples. The oxygen ion transport number of the samples increases with increasing temperature. SOFCs results show that PrGa0.9 Mg0.1 O3 has the best properties, for which the power density of 0.131 W/cm2 and the short circuit current density of 0.45 A/cm2 were achieved at 940 ℃. This study reveals that Mg doped PrGaO3 is a kind of solid electrolyte with superior properties.
    Synthesis and Structure of Novel Trinuclear and Tetranuclear Ruthenium Carbonyl Clusters Containing μ3-P orμ3-PR and μ3-S Bridging Ligands
    NING Bao-Zhu, WU Bing-Fang, LIU Shu-Tang, HU Xiang
    2001, 22(8):  1286-1289. 
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    The reaction of [Ru3(CO)12 ] with dimer of p-methoxyphenyl thionophosphine sulfide in THFyields the novel trinuclear ruthenium carbonyl cluster [( μ-H)] 2Ru3(CO)9( μ3-P)](Ⅰ) and tetranuclear ruthenium carbonyl cluster (Ⅰ) and tetranuclear ruthenium carbonyl cluster [Ru4(CO)10 ( μ3-PC6H4OMe)](Ⅱ). These clusters were characterized by elemental analysis, IR, 1H NMR, 31P NMRand MSspectrometric methods and the molecular structure of compound Ⅰ was determined by X-ray diffraction analysis. The molecular geometry of compound Ⅰ contains a trigonal pyramid Ru3Pskeleton with a Ru3 triangle at the base and the nude phosphorus atom as a 5e μ3-Pbridging ligand at the apex. Though compound Ⅰ is one with 49 valence eletron, its Ru-Ru distances(average 0.2830 nm) are astonishly short and compound Ⅰ is rather stable in the exposure to oxygen and moisture. The structure of compound Ⅱ is believed to have a tetrahedral Ru4 core which is attached to a μ3 Sand a μ3-PC6H4OMe ligand on tetrahedron's two triangular faces.
    Hydrothermal Synthesis and Crystal Structure of a Novel Layered Compound [Ni(C10H8N2)2V3O8.5]
    LUAN Guo-You, WANG En-Bo, HAN Zheng-Bo, LI Yang-Guang-LU Ying, HU Chang-Wen, HU Ning-Hai, JIA Heng-Qing
    2001, 22(8):  1290-1291. 
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    Anovel layered compound, [Ni(C10 H8N2)2V3O8.5], was hydrothermally synthesized and structurally characterized by single crystal X-ray diffraction. The compound crystallizes in monoclinic system, space group P21/c with a=15518(3)nm, b=14761(3)nm, c=10483(2)nm, β=9202(3)°, V=23998 (8)nm3, Z=4, R=00467, wR2=00859.
    Structure and Properties of Dibridged (μ-oxo)(μ-CO3) diiron(Ⅲ) Complex
    YAN Shi-Ping, WANG Qing-Lun, CHENG Peng, LIU Xin, LIAO Dai-Zheng JIANG Zong-Hui, LENG Xue-Bing, WENG Lin-Hong
    2001, 22(8):  1292-1294. 
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    A ( μ oxo)( μ-CO3)diiron(Ⅲ) complex of tri(2-pyridylmethyl)amine(TPA), [Fe2L2( μ-O) ( μ-CO3)] (ClO4)2·MeOH·EtOH·H2O], was synthesized and characterized, where Lrepresents TPA. This complex crystallizes in the monoclinic space group P21/c with a=1.1810(3)nm, b=3.7281(8)nm, c=1.3770(3)nm , β=115.393(3)°, V=5.477(2)nm3, Z=4. R1=0.0849 and wR2=0.1962. The UV-Vis spectra of this compound show multiply absorption bands in200-800 nm range, which are similar to that of N3- coordinated met hemerythrin. , was synthesized and characterized, where Lrepresents TPA. This complex crystallizes in the monoclinic space group P21/c with a=1.1810(3)nm, b=3.7281(8)nm, c=1.3770(3)nm , β=115.393(3)°, V=5.477(2)nm3, Z=4. R1=0.0849 and wR2=0.1962. The UV Vis spectra of this compound show multiply absorption bands in 200-800 nm range, which are similar to that of N3- coordinated met hemerythrin.
    Synthesis, Structure and Electrochemistry of Copper(Ⅱ) Complexes with Di[( o-salicylidenimino)phenoxy]ethane Ligand
    ZHANG Wen-Xing, SI Shu-Feng, MA Chang-Qin
    2001, 22(8):  1295-1297. 
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    Two Cu(Ⅱ) complexes with title Schiff-base ligand H2L, micro-crystal Cu(HL)ClO4·H2Oand single crystal , have been synthesized and characterized by IRspectra, etc .. By cyclic voltammetry, a quasi-reversible electron-transferring process has been shown in Cu(Ⅱ)/Cu(Ⅰ) couples reaction of [CuL]; the given value E1/20=-0.73 Vhas been estimated. The structure of [CuL] has been determined by X-ray diffraction with R=0.036. The results indicate that the deprotonic ligand, as a practically tetradentate, coordinates only with its two imino and two phenoxo groups to form a D2d symmetric geometry. Two different torsional modes of the homologous ligands, occurring in mono-and di-nuclear Cu(Ⅱ) complexes, respectively, have been contrasted and discussed.
    Induction Effect of Ca2+ on Ion-channel Behavior of Supported Phospholipid Membranes
    HAN Xiao-Jun, SONG Yong-Hai, WU Zheng-Yan, ZHANG Bai-Lin, WANG Er-Kang
    2001, 22(8):  1298-1300. 
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    As a kind of supported bilayer lipid membranes, hybrid bilayer membrane(HBM) was applied to the interaction between Ca 2+ and lipid for the first time. By using Fe(CN)63- as a probe, we found that Ca 2+ coulDInduce the ion channel of HBMto be in open state. STMimages study proved this phenomenon.
    Determination of Cadmium at Ultra-trace Level by FI Cold Vapor Generation AAS with On-line Ion Exchange Preconcentration
    YAO Bo, XU Shu-Kun, FANG Zhao-Lun
    2001, 22(8):  1301-1304. 
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    Amethod for the determination of cadmium by flow injection cold vapor generation atomic absorption spectrometry(FI-CVGAAS) with an on line ion exchange micro column preconcentration system was developed using IRC718, 122 and Muromac A-1 resin. The interferences from coexisting elements were studied. The detection limit(3σ) was 2.3-3.0 ng/Lwith a sampling frequency of 45-60/h. The precision was 2.0%-2.6% RSD( n=11) at 0.2 μg/Llevel. The method was applied to the analysis of water samples. Satisfactory recoveries of cadmium in reservoir water, tap water and brine waters were obtained for spiked samples.
    A Novel Piezoelectric Immunosensor for the Determination of Transferrin
    WANG Hua, WU Zhao-Yang, SHEN Guo-Li, YU Ru-Qin
    2001, 22(8):  1305-1309. 
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    Based on plasma-polymerized film(PPF) and polyelectrolyte, a novel piezoelectric immunosensor is developed for the determination of transferrin in human serum. The approach begins with the preparation of PPFon the surface of quartz crystal microbalance(QCM) by the glow-discharge. Through strong electrostatic attraction, a negative-charged polyelectrolyte which serves as a removable layer for the QCMreproduction is then self-assembled on the film, and positive-charged antibodies which specifically react with antigens are subsequently immobilized on the self-assembled layer by controlling the pHvalue. The effects of experimental conditions including the self-assembly of polyelectrolyte, the incubation of transferrin antibodies and the test of immunoreaction are discussed, respectively. In addition, the sensitivity, selectivity, regeneration and reproducibility of the immunosensor are investigateDIn detail. Under the optimal experimental conditions, the QCM immunosensor can be used to determine quantitatively transferrin in human serum with the linear range of 0.10-12.65 μg/mL. It is found that the results of clinical samples by this developed method are identical to those by the ELISAmethod.
    Electrochemical Behavior and Application of Pirarubicin at Co Ion Implantation Modified Ultramicroelectrode
    MAO Yan-Ning, HU Jing-Bo, LI Qi-Long, XUE Ping
    2001, 22(8):  1310-1314. 
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    With Co ion implantation modified carbon fiber ultramicroelectrode as the working electrode, in0.1 mol/L HAc-NaAc(pH=5.05) buffer solution, a sensitive reductive peak of pirarubicin was obtained by linear sweep voltammetry. The peak potential was-0.520 V( vs . SCE). The peak current was proportional to the concentration of pirarubicin over the range of 1.0×10-7 6.0×10-6 mol/L, with a detection limit of 5.0×10-8 mol/L. This method has been developed for the determination of pirarubicin in human urine. The recoveries were in the range from 91.6% to 106.7%. The experiments showed that the reduction process of pirarubicin was a reversible process with adsorption. The composition and depth distribution of elements on the surfaces of Co ion implantation modified carbon fiber microelectrode were determined by scanning electron microscope and Auger electron spectroscopy. The experiments showed that Co was surely implanteDInto the surface of carbon fiber, and the implanted Co catalyzed the reduction of pirarubicin.
    Liquid Membrane Transport of Transition MetaLIons with Calix Crowns
    MA Hui-Min, WANG Zhi-Hua, ZHENG Qi-Yu, WEN Li-Quan-MA Quan-Li, SU Mei-Hong, HUANG Zhi-Tang
    2001, 22(8):  1315-1318. 
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    Selective transport of metaLIons across liquid membrane can be achieved by using calixarene derivatives with recognition groups. Four new calix[4] crowns, in this work, were examined for the transport of transition metaLIons such as Cu 2+ , Fe 3+ , Co 2+ , Ni 2+ and Zn 2+ . It was found that one of these calix crowns, 25,27-dihydroxy-26,28-(3',6'-dioxa-2',7'-dioxooctylene)dioxycalixarene (Ⅲ), transported efficiently Cu 2+ . Various factors affecting the transport of Cu 2+ with Ⅲ were investigateDIn detail, including source phase and receiving phase's acidities, carrier concentration, time, temperature, etc .. The mechanism of H+ exchange was suggested for the present system H2O-(liquid membrane)-H2O, and the transport process of Cu 2+ was briefly discussed.
    Estimation of Rank by Chemical Subspace Invariant to Linear Transformation Method
    TAN Yong-Xi, JIANG Jian-Hui, XIE Hong-Ping, LIANG Yi-Zeng, YU Ru-Qin
    2001, 22(8):  1319-1322. 
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    Based on the invariability of the sought-for chemical subspace to the linear transformation, a novel approach, called chemical subspace invariant to linear transformation method, is developed for estimation of chemical rank of two way data matrices. The idea of this approach is that the chemically meaningful subspace is the most stable one with respect to the linear transformation of the two-way data along one order. Two quantitative indexes, projection residual as well as included angle of subspace, are also proposed to measure the difference of two subspaces. The results of two NIRdata show that this method provides a very promising tool for chemical rank estimation of two-way data matrices.
    Studies on Negative Electrospray Ionization Mass Spectrometry on Saponins
    CUI Meng, LIU Zhi-Qiang, SONG Feng-Rui, LIU Shu-Ying
    2001, 22(8):  1323-1325. 
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    Two kinds of saponins have been investigated by negative electrospray ionization(NESI) mass spectrometry. Under ESIconditions, the [M-H]- ions of saponins were observed which provide the molecular weights of saponins. The fragment pathways of - ions of these two saponins depend on their structures. For steroidic saponins, [M-H]- ion only produces the fragment ions by the losses of sugar units. For oleanolic saponins, [M-H]- ion yields the cross ring ions as well as the fragment ions by the losses of sugar units. Moreover, the abundance of the former is higher than that of the latter. The characteristic fragments are used to provide the sequence and some linkage information of sugar moieties of saponins. Especially, their fragment difference strongly depends on the linkage between the aglycone and the sugar moieties.
    The Asymmetric Oxidation of Sulfides Catalyzed by Chiral Oxazoline-Ti(Ⅳ) Complexes
    PENG Yun-Gui, FENG Xiao-Ming, CUI Xin, JIANG Yao-Zhong
    2001, 22(8):  1326-1331. 
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    Aseries of new chiral oxazoline-Ti(OiPr)4 complexes were synthesized, which were firstly and successfully applied to the catalytic asymmetric oxidation of sulfides and resulteDIn chiral sulfoxides. The reactivity and enantioselectivity were strongly influenced by the structure of the oxazolines. When (4S,5S )-4,5-dihydro-4,5-diphenyl-2-(2'-hydroxy-3'-tert-butylphenyl) oxazoline was used as the ligand, 2.0 mol of TBHPwas useDIn the oxidation of methyl phenyl sulfide, the sulfoxide was obtaineDIn96% e.e. . The influence of solvent, amount of catalyst, counterion and other conditions on the reaction was also investigated.
    The Stereoselectivity of the Amidation Catalyzed by Lipase
    YANG Bo, IZUMI Taeko, ZHANG Shu-Sheng
    2001, 22(8):  1332-1337. 
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    An empirical rule for amidation of amines which contains chiral carbon catalyzed by lipase from candida antrarctica has been proposed, anDIt is the same one as alcohols. It can be used to predict that which enantiomer reacts faster based on the relative sizes of the substituents at the stereocenter, but the recognization is very delicate to the structure of the carbon contacted with amino group. The R-enantiomer reacts faster when the amines are secondary amines; the Senantiomer reacts faster when they are primary amines.
    The Chemical Constituents from Anemone Rivularis
    LIAO Xun, LI Bo-Gang, WANG Ming-Kui, DING Li-Sheng
    2001, 22(8):  1338-1341. 
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    Eight compounds were isolated from the methanol extract of the roots and aerial parts of Anemone rivularis Buch.-Ham. ex DC. By means of spectroscopic methods, their structures were established as oleanolic acid 3 O α Larabinopyranoside(1), oleanolic acid 3-O-α-Lrhamnopyranosyl(1→2) α-Larabinopyranoside(2), oleanolic acid 3-O-α-Dribopyranosyl(1→3) α-Lrhamnopyranosyl(1→2) α-Larabinopyranoside(3), hederaginin 3 O-α-Larabinopyranoside(4), 3-O-α-Dribopyranosyl(1→3) α-Lrhamnopyranosyl(1→2) α-Larabinopyranosly oleanolic acid 28 O-α-Lrhamnopyranosyl(1→4) β-Dglucopyranosyl(1→6) β-Dgulcopyranoside(5), 3-O-α-Dribopyranosyl(1→3) α-Lrhamnopyranosyl(1→2) α-Larabinopyranosly hederaginin 28 O-Lrhamnopyranosyl(1→4) β-Dglucopyranosyl(1→6) β-Dgulcopyranoside(6), 3β,12β,23-trihydroxy olean 28,13 β-olide(7) and 3β,12β,13β-trihydroxy olean 28 oic acid 3-O-Dribopyranosyl(1→3) α-Lrhamnopyranosyl(1→2) α-Larabinopyranoside(8)-respectively. The last two compounds were new ones and named anemonolide(7) and anemoside B(8).
    Progress in the Study on Peptide Synthesis Catalyzed by Immobilized Enzyme
    LIU Ping, TIAN Gui-Ling, YE Yun-Hua
    2001, 22(8):  1342-1348. 
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    The review deals with the factors which have influence on peptide synthesis catalyzed by immobilized enzyme anDIts application for peptide synthesis. Particular attention is paid to important effect factors, such as solvent, support, pHvalue, etc . and the reasons for these effects are discussed. Immobilized enzymes applied to peptide synthesis, i.e., sweetener aspartame, enkephalin and other bioactive peptides and so on, were briefly summarized.
    Studies on the Cleavage of Bovine Serum Albumin by Ser-His
    CHEN Jing, WAN Rong, LIU Hai, JIANG Yu-Yang, ZHAO Yu-Fen
    2001, 22(8):  1349-1351. 
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    It has been found that Ser-His could cleave bovine serum albumin(BSA), with the most suitable pHaround 6.0. The kinds of buffers have different influences on the cleavage activity. The phosphate buffer and BRbuffer are the most effective. The hydroxyl group of the serine residue is the essential functional group for the cleavage, while the amide bond, imidazole, and carboxyl group of Ser-His increase the cleavage activity.
    A Novel Synthetic Method of Hydratropic Aldehyde
    SHI Zhen, LU Lin-Gang, WANG Yun-Xia
    2001, 22(8):  1352-1354. 
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    Based on the one carbon unit transfer reaction of tetrahydrofolate coenzymes, hydratropic aldehyde was synthesized successfully by using benzimidazolium salt as tetrahydrofolate coenzyme model at formic acid oxidation level and Grignard reagent as a nucleophile to which one carbon unit was transfered. Anovel method for the preparation of hydratropic aldehyde was provided. The mechanism for the addition-hydrolysis reaction of benzimidazolium salt with Grignard reagent and the effects of reaction condition on the yield are discussed.
    Quantum ChemicaLInvestigation of Silicon-sulfur Clusters[(SiS2)nS]-(n=1～4)
    WANG SU-Fan, FENG Ji-Kang, SUN Chia-Chung, LIU Peng, GAO Zhen, KONG Fan-Ao
    2001, 22(8):  1355-1358. 
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    The possible geometrical structures and relative stability of silicon sulfur clusters [(SiS2)n S]- ( n=1-4) are explored by means of density functional theory(DFT) quantum chemical calculations(B3LYP/63-1+-G*). The effects of polarization functions and electron correlation are includeDIn these calculations. The electronic structure and vibrational spectrum of the most stable geometrical structure of [(SiS2)n S]- are analyzed by the same method. As the result, the regularity of the [(SiS2)n S]- cluster growing is obtained, and the calculation can be used to predict the mechanism of the [(SiS2)n S]- cluster forming.
    Quantum Chemical Studies of Metal-metaLInteraction and Properties of complex [Ti(CO)6(MPEt3)]- (M=Au,Ag,Cu)
    SU Zhong-Min, HU Li-Hong, CHU Bei, QIU Yong-Qing, WANG Rong-Shun
    2001, 22(8):  1359-1363. 
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    The stability of [Ti(CO)6(AuPEt3)]- was studied systematically by using ab initio HFand density functional theory(DFT) B3LYPmethods. The molecular structures of calculation were in agreement with the XRDcrystal data. The basis set superposition error (BSSE) was corrected by the counterpoise method, the interaction energy of Ti-Au was 10.8575 eV (B3LYP/BSSE). Electronic properties and regularities of interaction in [Ti(CO)6(MPEt3)]- (M=Au, Ag, Cu) centered by Cu group elements were discussed. The calculation results showed that [Ti(CO)6(AuPEt3)]- was the most stable in the complexes of Cu group, and the interaction of metal metaLIn it was striking.
    A Theoretical Simulation of Hydroboration of Alkenes with BH3 in Ether Media
    FAN Yu-Bo, DING Zong-Biao, WANG Quan-Rui, TAO Feng-Gang
    2001, 22(8):  1364-1367. 
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    The reaction of the monomeric BH3 with alkenes in ether media has been examined by using B3LYP, a hybrid density functional method, with 631G* basis set. Calculations of various possible species involveDIn the hydroboration process, including the complexes of borane (BH3) with dimethyl ether, ethylene, propene, 1-butene, trans-2-butene, cis-2-butene, 2-methylpropene, 2-methyl 2-butene and 2,3-dimethyl-2-butene as well as the reactants and transition states of the corresponding hydroboration have been performed. The zero point energies(ZPE) and thermal analyses were computed at the same level. Based on the calculations, the prior formation of a three center π-complex intermediate of BH3 with the respective alkene is predicted and the overall reaction rate was determined. For the formation of the π-complex intermediates, two extreme pathways, i.e . the SN1 and SN2-like manner, have been compared, with the latter one more preferentially in terms of the activation barrier by 2528 kJ/mol endothermically.
    Surface Enhanced Raman Spectroscopic Detection of Porphyrin Monolayer
    ZHU Zi-Hua, SHENG Xiao-Xia, ZHANG Zhi-Jun, ZHU Tao, LIU Zhong-Fan
    2001, 22(8):  1368-1372. 
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    Using4 mercaptopyridine(4-MPy) self-assembled on gold substrate as coupling agents, monolayer of cobalt(Ⅱ)-5,10,15,20-tetrakisphenyl-porphyrin (CoTPP) was fabricated on the pyridinyl-ter minated surface. Further deposition of Au nanoparticles enables the detection of CoTPPmolecules in monolayer to be possible by Surface Enhanced Raman Spectroscopy. The red-shift of "structure sensitive" peaks of porphyrin ring indicates the existence of chemicaLInteraction between CoTPPmolecules and the pyridine terminals, which was believed as the coordination between the nitrogen atom of pyridine ring and the cobalt atom in CoTPP. From the orientation of 4-mercaptopyridine SAMs, it can be deduced that the CoTPPmolecules are approximately parallel to Au substrate in the above structure.
    Electrochemical Characterization on the Interaction Between Hemoglobin and NO Molecule
    LI Qing-Wen, GAO Hong, HUANG Hao, WANG Yi-Ming, FENG Jun, LUO Guo-An
    2001, 22(8):  1373-1375. 
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    Nanocrystalline TiO2 particles film has been considered as an eminent matrix for the immobilization of biomolecules due to its high biocompatiability, high protein loading and special binding ability. The direct electron transfer process of hemoglobin was achieved at nanosized TiO2 film electrode, in which a well-defined redox peak of hemoglobin could be observed. However, this peak decreased with the presence of NO, indicating the electrochemical activity of hemoglobin was inhibited by the interation between hemoglobin and NO. While the further evidence revealed that such activity could be recovered after releasing NOfrom hemoglobin with electrochemical oxidation method.
    The Behavior of Photo-generated Charge Transfer of Dimeric Porphyrin
    XIE Teng-Feng, WANG De-Jun, ZHAO Zhi-Xin, XU Jin-Jie, ZHU Lian-Jie, LIU Guo-Fa, LI Tie-Jin
    2001, 22(8):  1376-1378. 
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    The photovoltaic properties of dimeric porphyrin have been studied by means of surface photovoltage spectrum(SPS) and fielDInduced surface photovoltage spectrum(FISPS). The results show that a negative SPVresponse band(P) appears in the long-wave region which takes on n type character and the π-π * transition band takes on p type character. Pband disappears under high vacuum and appears under O2 atmosphere. The photo-charge-transfer process generated between π-π * transition band of dimeric porphyrin and Pband, which has been attributed to the photo adsorption and photo desorption of O2 on the surface of dimeric porphyrin.
    Relationship Between Chemical Components of Surface Coatings and the Maximum Adsorption of Cd and Pb by Surface Coatings DevelopeDIn Natural Waters
    DONG De-Ming, LI Yu, HUA Xiu-Yi, ZHANG Jing-Jing
    2001, 22(8):  1379-1381. 
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    Adsorption of Cd and Pb to components of surface coatings developeDIn five natural waters(Jilin Province, China) was carried out. The result indicates that the content of Fe oxides on surface coatings is much higher than that of Mn oxides. Langmuir isotherm is more suitable to describe the adsorption of Cd and Pb onto surface coatings. The maximum adsorption of Pb and Cd to surface coatings is directly proportional to the contents of Mn oxides and Fe oxides on surface coatings with significant correlation( n=5, α=0.01), respectively, and to the content of aluminum oxides with significant correlation (n=5, α=0.05), highlighting the relative importance of metal oxide fraction for Pb and Cd adsorption to the surface coatings developeDIn the five natural waters. The result agrees with that previously obtained by selective extraction technique for the relative importance of Fe and Mn oxides and organic materials in controlling Cd and Pb adsorption to surface coatings developeDIn Cayuga Lake(New York, USA).
    Active Surface Structure of AgMoO2PO4·MoO3 Catalyst for Selective Oxidation of Propane
    ZHANG Xin, WENG Wei-Zheng, WAN Hui-Lin
    2001, 22(8):  1382-1384. 
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    The active surface structure of AgMoO2PO4·MoO3 catalyst was investigated by in situ confocal microprobe Raman spectroscopy, evaluation of catalytic performance, XRDand XPStechniques. The results show that MoO3 and [Mo7O24 ] 6- may be reconstructed to [Mo6O19 ]2- under the reaction conditions. The structure change only occurred on the catalyst surface, and thus [Mo6O19 ]2- may be an active dynamic surface structure responsible for the better catalytic performance of selective oxidation of propane.
    New Approaches to Immobilization of Aluminium Chloride on γ-Al2O3
    CAI Tian-Xi, HE Min, SHI Xian-Zhe, SONG Zhao-Xia, CAO Dian-Xue
    2001, 22(8):  1385-1387. 
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    The method of preparation of AlCl3 catalyst immobilized on γ-Al2O3 was investigated. AlCl3 generated by reacting CCl4 with pure γ-Al2O3 at 500℃ and γ-Al2O3 with bimodal meso-and macro-pore structure were used as immobilizing agent and support, respectively, to prepare the catalyst. The effect of various factors of immobilization conditions on catalytic property in isobutene polymerization was examined. The catalyst, in which the mass fraction of AlClx is about 7.5 and x=2.2, showed a high activity, selectivity and stability, and no considerable differences in the catalytic behavior were founDIn the following ranges: reaction temperature, 300-400 ℃; reaction time, 0.5-4.0 h; flow of CCl4 of adding, 1.15-2.01 mL/h for 15 mL γ-Al2O3. Additionally, it was shown that the catalytic property in isobutene polymerization is not only dependent on the nature of support, but also on its geometric structure. Compared with the catalysts having micro-porous and meso-porous structure which showed a poor stability, the catalyst with meso-and macro-pore bimodal structure exhibited a very high stability, and was supposed to be most suitable one, anDIt was ascribed to that in the case of the latter, harmfuLInfluence of intraparticle diffusion caused by "pore clogging" of large product molecules in the pore channel effectively reduced.
    Studies on the Kinetic Properties of Cells of Aquatic Animals During Death with 31P NMR
    WANG Tian-Zhi, DU Fei, MAO Xi-An
    2001, 22(8):  1388-1390. 
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    Cell death manner is related to the contents of intra-cell energy substances. The rate constants and the half life-time of ATP, phosphocreatine (PCr) anDInorganic phosphorus (Pi) in different cells of eel and crucian during their death have been determined with 31P NMR. It has been found that there are differences in rate constants and change rule of these energy substances for different animals and different cells in the same animal from this study. The decreasing order of the half life time is: muscle of eel>brain of eel>muscle of crucian for ATP; brain of eel≈muscle of eel>muscle of crucian for PCr. These results are very vital to understanding the concerned change pattern of energy substances and the speed of cell death.
    Density Functional Studies of the Chemisorption of CO on Transition Metal Catalysts of Ru, Rh, Pd(Ⅰ)
    SUN Ren-An, LIU Yong-Dong, WANG Chang-Sheng
    2001, 22(8):  1391-1393. 
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    Using the M4(M=Ru, Rh, Pd) clusters as models, chemisorption of COat the top and bridge sites has been performed by Gaussian programs, at the DFT/LANL1DZlevel. Metal-CObonding and the influence of CObond after chemisorption COhave been studied, and the effects on the products of COhydrogenation have been inferred. The calculations have shown that all the CObonds are wakened after adsorption. Ru catalyst weakens C-Obond the most largely, Pd weakens C-Obond the least, and Rh lies between them. So it could be concluded that the products of COhydrogenation have a trend to the hydrocarbons over the Ru catalyst, and the products are inclined to oxygenate over Pd, while there isn't obvious trend to the hydrocarbons and oxygenate on Rh.
    Preparation and Characteristics of Perylene Nanocrystals
    JI Xue-Hai, FU Hong-Bing, CAO Ya-An, XIE Rui-Min, ZHANG Xin-Tong, YAO Jian-Nian
    2001, 22(8):  1394-1396. 
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    Perylene nanocrystals with different sizes(10-250 nm) were prepared by reprecipitation. Compared with the absorption spectrum of perylene acetone solution, a new J-aggregate absorption peak appeareDIn the absorption spectra of nanocrystals. With the decrease of perylene nanocrystals' size, it shows a blue-shift in the absorption spectra. This blue-shift is due to the size dependent property. The perylene concentration of initial acetone solution or the amount of solution injecteDInto water, the aging time of organic nanocrystal dispersion and the adding of surfactant were the influencing factors of nanocrystal growth. We can gain the required microcrystals of different sizes by controlling the conditions of growth.
    A Kind of CdSNanocluster with Free Carboxyl Groups on Its Surface
    JIANG Lin, CHEN Xia, YANG Wen-Sheng, JIN Jian-YANG Bai-Quan, XU Li, LI Tie-Jin
    2001, 22(8):  1397-1399. 
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    CdSnanoclusters were directly synthesizeDIn aqueous solution by using mercaptoacetic acid as the stabilizer. The results of TEM(Transmission Electron Microscopy) and ED(Electron Diffraction) show that the structures and aggregations of the resulting CdSnanoclusters can be affected by the molar ratio of mercaptoacetic acid and Cd 2+ ion. When the ratio was high, the resulting nanoclusters were observed as densely packed layer structure on the template. When the ratio was low, the prepared CdSnanoclusters can not form highly aggregated structure. Fluorescence spectra of the CdSnanoclusters show a strong yellow fluorescence.
    Synthesis and Characterization of Zeolite FSM-16 and TiO2/FSM-16
    ZHOU Qun, SUN Fang, CHUAI Bing-Jie, GU Jian-Sheng
    2001, 22(8):  1400-1402. 
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    Zeolite FSM-16 was synthesized by reconstruction of layered silicate in the presence of organic surfactant. With partial replacement of Ti 3+ with organic cations, TiO2 nano-structured particles were simultaneously built in the channel of the zeolite as the framework of the zeolite was formed. XRD, IRand Raman spectroscopic characterizations indicate that SiO4 tetrahedron may be distorted and transferred from Q 3 to Q 2 form due to the pucker and reconstruction of the layered structure. The formation of TiO2 nano structured particles had no influence on the formation of zeolite framework, however, the interaction obviously occurred between TiO2 nano structured particles and zeolite framework.
    Studies on the Room Temperature Conductivity of PEO-LiClO4-Al2O3 Composite Polymer Electrolyte
    GU Ning-Yu, QIAN Xin-Ming, CHENG Zhi-Liang, JIANG Jun-Guang, YANG Xiu-Rong, DONG Shao-Jun
    2001, 22(8):  1403-1405. 
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    Acomposite polymer electrolyte of Polyethylene oxide (PEO)-LiClO4 containing fine Al2O3 particles was studied by using differential scanning calorimetry, infrared spectroscopy and electrochemicaLImpedance spectroscopy. Compared with the polymer electrolyte without Al2O3 particles, the glass transition temperature and the degree of crystallinity were decreased, and the room temperature conductivity of PEO-LiClO4 Al2O3 composite polymer electrolyte was considerably enhanced. Moreover, the equivalent circuits and the effect of dc potential on impedance spectroscopy were discussed.
    Studies on the Technique and Mechanism of Solid Grafting Polypropylene with Dual Monomers
    ZHANG Li-Feng, GUO Bao-Hua, ZHANG Zeng-Min
    2001, 22(8):  1406-1409. 
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    Solid grafting is a promising grafting method, which is simple, cheap and easy to control, to get a polar polypropylene(PP). However, the achieved product may have a severe degradation and the graft ratio cannot satisfy us. In this paper, dual monomers, maleic anhydride(MAH) and tri-allyLIsocyanurate(TAIC) were used to graft onto PP. It was found that TAICwas efficient to enhance the MAHcontent of the products and prohibit PP's degradation. The MAHcontent of the product can reach 7.2% with 4%TAIC. This is prominent when it was compared with melt grafting product and normal solid grafting product. The MAHcontent and the melt flow rate(MFR) of the product can be adjusted by changing TAIC's amount. The reaction mechanism of dual monomers in the grafting polymerization and their composition in the product were also discussed.
    Crystalline Characters of Modified Hyperbranched Polyester
    KOU Hui-Guang, ZHU Sheng-Wu, SHI Wen-Fang
    2001, 22(8):  1410-1413. 
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    To obtain a new kind of resin for practical UVcurable powder coating systems, hyperbranched polyester, BoltornTM H20, was modified with octadecyLIsocyanate (or palmitoyl chloride) and acryloyl chloride, thus resulting in an UVcurable resins with crystalline molecular shell and amorphous interior. The high melting point( Tm) can be resulted largely by the crystalline area of the crystallizable moieties. The degree of crystallinity is higher with more crystallizable moieties. As a result, Tm of the resin modified with octadecyLIsocyanate is higher than that of one modified with palmitoyl chloride. The hyperbranched polyester BoltornTM H20 modified with octadecyLIsocyanate maybe used for powder coating systems.
    Reactive Reinforcement of the Interface of High Performance Polymer Blends by PMR-POI
    LAI Ming-Fang, YANG Yu-Ming, LIU Jing-Jiang
    2001, 22(8):  1414-1418. 
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    The effect of PMRpolyimide(POI) as the interfacial agent on the interface characteristics, morphology features and crystallization of poly(ether sulfone)/poly(phenylene sulfide)(PES/PPS) and poly(ether ether ketone)/poly(ether sulfone)(PEEK/PES) partly miscible blends were investigated by means of the scanning electron microscopy, WAXDand XPSsurface analysis. It is found that the interfacial adhesion was enhanced remarkably, the size of the dispersed phase particles was reduced significantly and the miscibility was improved by the addition of POI. During melt blending cross link and/or grafting reaction of POIwith PES, PEEKand PPShomopolymers was detected, however the reaction activity of POIwith PPSwas much higher than that of PESand PEEK. It was also found that POIwas an effective nucleation agent of the crystallization of PPS.
    The Interfacial Compatibilization for PSF/LCP Blends by a Maleic Anhydride Modified Polysulfone
    ZHANG Jun, HE Jia-Song
    2001, 22(8):  1419-1424. 
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    Maleic anhydride-grafted polysulfone(PSF-g-MAH) was prepared. Compared to polysulfone, the surface tension anDIts polar fraction of PSF-g-MAHwere increased by modification. The PSF-g-MAHwas used to compatibilize polysulfone(PSF)/liquid crystalline polymer(LCP) blends. The processabilities and the interfacial properties of PSF/LCPblends before and after compatilization were investigated. It was found that the melt viscosities were increased by the addition of PSF-g-MAH. DRS-FTIRinvestigations showed that the speciaLInteraction between PSFand LCPphases was increased due to the incorporation of PSF-g-MAH. The XPSand PLMstudies revealed that some chemical reactions had occurred between mPSFand LCPphases, which produced PSF-VBcopolymers. It is suggested that the compatibility is attributed to some interactions including both chemical and physical ones. Amodel to illustrate the compatibilization of mPSFin PSF/VBblends has been proposed.
    In-situ FTIR Spectroscopic Study on the Conformational Change of Isotactic Polypropylene upon Heating
    ZHU Xin-Yuan, FANG Ya-Peng, LI Yong-Jin, YAN De-Yue, ZHU Pin-Fang, LU Qing-Hua
    2001, 22(8):  1425-1427. 
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    The experimental data obtained from fast heating FTIRspectroscopy have confirmed that a conformational change occurs at about 135 ℃ for semicrystalline iPP. Based on the results of density and WAXDmeasurements, it can be inferred that the conformational change occurring at 135 ℃ comes from the disordering of helical sequences in non-crystalline phase, which is further corroborated by the FTIRstudy on the chloride polypropylene.
    Structures of 2D Ordered Monolayer of Rigid Cyclic Oligomer
    BEN Teng, CHEN Chun-Hai, SUN Hui, CAO Hui, YU Kun-Qian, LIU Xin-Cai, WANG Xing, QIU He, WU Zhong-Wen, ZHANG Wan-Jin, XIA Qing-Tao, WEI Yen
    2001, 22(8):  1428-1430. 
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    The spreading behavior of new type of chiral and achiral rigid cyclic oligomer on the water surface was investigated by measuring the surface pressure(π)-area( A ) isotherms, with the aim of comparison of new type LBfilms of chiral and achiral rigid cyclic oligomers. Molecular resolution atomic force microscope images of the Langmuir-Blodgett(LB) film was observed and the structure of their two-dimensional crystals on the basal plane of mica was studied.
    Synthesis of Poly[styrene(iodoso diacetate)] and Application in Regeneration of Carbonyl Compounds from Semicarbazones
    ZHANG Ji-Zhen, ZHU Qing, HUANG Xian
    2001, 22(8):  1431-1433. 
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    The 2% cross-linked poly[styrene(iodoso diacetate)] was synthesized, which was used as oxidative reagent from semicarbazones of ketones to the corresponding ketones in wet acetonitrile under mild conditions, and the possible mechanism was discussed.
    Tribological Properties of PVA Hydrogels and 2-Hydroxyethyl(meth)acrylate Hydrogels
    GUO Xing-Lin, LI Fu-Mian
    2001, 22(8):  1434-1436. 
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    PVAhydrogels with different crystallinities obtained by varying freeze/thawed process cycles, as well as 2-hydroxyethyl methacrylate(HEMA) and 2-hydroxyethyl acrylate(HEA) hydrogels sheets crosslinked by polyethylene glycol dimethacrylate(PEGDMA-16) were prepared. The slide frictional properties of these hydrogels had been studied. It is found that the frictional behavior of these hydrogels do not obey Amonton's law due to the hydrodynamic lubrication mechanism caused by the squeezed water from the surface of hydrogels. When the loaDIncreased, more free water is squeezed out from the surface of hydrogels, thus the frictional coefficient is decreased. When the PVAhydrogels are exposed to air, the evaporation of the free water on the surface of hydrogels causes the increase in the frictional coefficient of PVAhydrogels. Additionally, with the increase of crystallinity of PVAhydrogels or crosslinking density of HEA, HEMAhydrogels, the network lattice of hydrogels becomes smaller, the water is difficult to squeeze out, resulting in the increase of the frictional coefficient.
    Syntheses and Spectroscopic Study of Three Difunctional Photorefractive Model Molecules
    LI Feng, SUN Ming-Hao, LI Yao-Xian, WANG Jing-Yuan, TANG Xin-Yi
    2001, 22(8):  1437-1439. 
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    The syntheses and spectroscopic properties of three difunctional photorefractive model molecules ethyl[2-cyano 3-(9-ethylcarbazol-3-yl)]acrylate(ECEA), 2-(4-nitrophenyl)3 (9-ethylcarbazol-3-yl)-acrylonitrile(NPEA) and 9-ethylcarbazol-3-azo-(4-nitrobenzene)(ECAN) are reporteDIn this paper. The results indicate that the spectroscopic properties are influenced by the structure of three molecules and these molecules belong to p-type semiconductor.
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