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    24 June 1995, Volume 16 Issue 6
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    Articles
    Investigation on Phase Diagram of YbCl3-CaCl2-NaCl
    ZHENG Chao-Gui, PENG Shao-Qin
    1995, 16(6):  827-830. 
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    The phase diagram of YbCl3-CaCl2-NaCl ternary system has been investigated by means of DTA, It is found that there are 4 fields corresponding to the primary crystallization of YbCl2,CaCl2,NaCl and Na3YbCl6respectively and 5 univariant lines related to the secondary crystallization in this system.The two reactions occurred in this system are:
    Hydrothermal Synthesis and Characterization of MSn2(PO4)3(M=Na,K,NH4)
    XU Yue-Hua, FENG Shou-Hua, PANG Wen-Qin
    1995, 16(6):  831-835. 
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    Hydrothermal synthesis of MSn2(PO4)3(M=Na, K, NH4)compounds has been carried out at lower temperature,and their pure phases were easily obtained by hydrothermal crystallization. The compounds crystallize in rho. mbohedral form with a=0.8526(2)nm and c=2.247(4) nm for NaSn2(PO4)3, a=0.8366(1) nm and c=2.356(4) nm for KSn2(PO4)3, a=0.8330(l) nm and c=2.390(5)nm for NH4Sn2(PO4)3.The results of thermal analysis show that for Na and Kanalogues neither decomposition nor condensation took place up to ll00℃, whereas NH4Sn2(PO4)3could exist stably below 769℃,above this temperature it could be transformed to HSn2(PO4)3LiSn2(PO4)3and HSn2(PO4)3could not be prepared directly by hydrothermal method. Apossible explanation for this is given.
    Hydrothermal Synthesis and Characterization of a New Layered Potassium Phosphatoantimonate
    AN Yong-Lin, FENG Shou-Hua, LI Lian-Sheng, XU Ru-Ren, YUE Yong
    1995, 16(6):  836-839. 
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    Anew potassium phosphatoantimonate with composition of 4K2O·4Sb2O5·P2O5·8H2O was synthesized by hydrothermal method,and characterized by SEM,XRD,XPS, 31PMAS NMR,IR techniques.This compound has a layered structure,into which the amine can be intercalated,and the Kions can be exchanged.
    Preparation of Silica Aerogels by Supereritical Drying Technique
    CHEN Long-Wu, GAN Li-Hua, YUE Tian-Yi, LI Guang-Ming, WANG Jue, SHEN Jun
    1995, 16(6):  840-843. 
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    Silica aerogels were prepared by sol-gel process and supercritical drying technique.The effects of the pHvalue of solution on the gelation time and the density of the aerogel samples were studied.Through XRD, SAXS,TEM and some other experimental methods,the structure of silica aerogel samples was primarily investigated. The results show that the silica aerogels were coherent,non-crystalline,nanosized porous solids.The mean diameter of particles is about l0 nm.
    Synthesis of Y2O3:Eu Phosphors with the Method of Microwave Heating
    LI Yuan-Ying, DAI De-Chang, CAI Shao-Hua
    1995, 16(6):  844-846. 
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    It is the first report of using the microwave heating to synthesize powder crystal form Y2O3: Eu3+phosphors whose structure is a kind of cubic system with lattice parameter a=1.0607 nm,The phosphors have excitation spectra peak atλex=248.5nm,and emission spectra peaks atλex=611.5 nm. Under 254 nm excitation, the phosphors were measured by FMS-1 chromatic detector,and its chromatic coordinates are x=0.646,y=0.350 respectively. The relative luminescent brightness is about 70%,compared with the same standard phosphors.The particle size distribution was measured by SA-CP3 particle size analyzer,and its medium diameter is 3.90μm.
    Studies on the Coodination of Tb(Ⅲ) and Ca(Ⅲ)with Amino Acid Under the Physiological condition
    ZHAO Shu-Fu, WANG Zeng-Lin, LIU Qi-Min, NIU Chun-Ji, NI Jia-Zuan
    1995, 16(6):  847-849. 
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    Tb(Ca)-glycine,Tb(Ca)-alanine, Tb(Ca)-glycine-alanine systems were studied by potentiometry(37℃, I=0. 15 mol/L NaCl).The stability constants of complexes and distribution of species in ternary system were obtained.The results show Ca<Tb for the stability of binary complexes,Ca>Tb for the ternary complexes.The species convert each other with changing pHvalues.
    Determination of Vanadium, Niobium and Tantalum as Their 2-(2-Pyridylazo)-5-diethylaminophenol Chelates by Reversed-phase HPLC
    WANG Hong, ZHANG Hua-Shan, QIU Pei-Hong, CHENG Jie-Ke
    1995, 16(6):  850-853. 
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    Elements V,Nb and Ta have extremely similar chemical properties.They interference seriously with each other in their analysis,and it is difficult to determine the single element.In this paper,2-(2-pyridylazo)-5-diethylaminophenol(PADAP)is used as the precolumn derivative reagent for the first time and the simultaneous determination of V,Nb and Ta has been achieved in 11min at 580 nm on C18column with mathanol-water(50/50, V/V)containing 0.1%tartaric acid and l0 mmol/L pH=5 acetate buffer as the mobile phase.The detection limits are 0.34,0.29 and 7.30 ng/mL for V,Nb and Ta respectively when the ratio of signal to noise is 3.This method is sensitive and has been applied to the analysis of mineral.The results correspond with the certified values and the recoveries of 99.0%─101.1%are obtained.
    Fabrication and Electrochemical Characterization of Interdigitated Array Microband Electrode
    CAI Cheng-Xin, JU Huang-Xian, CHEN Hong-Yuan
    1995, 16(6):  854-858. 
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    The interdigitated array(IDA)microband electrode,which was made of 50 couples Au microelectrodes with 8 μm wide,4 μm gap and 500 μm long,was fabricated by using a photolithographic technique.The surface of IDAwas revealed with scan electron microscopy(SEM).The voltammetric characteristics of the IDAwas studied by means of cyclic voltammetry and chronoamperometry with four electrode configuration for generator collection mode and three electrode configuration for opened collector mode.Current-time curves for IDA in ferrocene dimethyl sulphoxide solution were subject to a quantitative comparison with the diffusion theory of microband electrode.The deviation between the theoretical and the experimental curves was discussed.The shielding factor, feed back factor and collection efficiency of IDA were determined.
    Resolution of Completely Overlapping Chromatographic Peaks by First Differentiation of Two-Way Data
    XU Jing, CUI Hui, HE Tao, LIANG Yi-Zeng, YU Ru-Qin
    1995, 16(6):  859-864. 
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    Anew approach to resolve completely overlapping chromatographic peaks is developed in this paper.Taking the advantage of different disappearing rates of two components,the method can obtain the approximate spectrum of embedded component by first differentation of two-way data.Applying the method to resolving the two-way chromatograms with two overlapping peaks of ascorbic acid and nicotinic acid,the estimated spectra accord well with the pure ones.The result is satisfactory.
    High Current and Microsecond Duration Pulsed Hollow Cathode Lamp Excited Inductively Coupled Plasma Atomizer Atomic Fluorescence Spectrometry
    GONG Zhen-Bin, YANG Peng-Yuan, WANG Xiao-Ru, HUANG Ben-Li
    1995, 16(6):  865-867. 
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    ICP-AFS excited by hollow cathode lamp(HCL)with high current(15A)and microsecond pulse(1.5μs)power supply has been studied.The detection limit(2σ)for Ca obtained with an 850 W ICP was 0.07 ng/mL,which was 40 times better than that obtained with conventionally pulsed(cp.)HCL excited at the same ICP power,and 30 times better than the best detection limit for cp.HCL,which was obtained with an 800 W ICP.
    The Application of Optimized Iterative Target Transformation Factor Analysis in Multicomponent FTIR Spectra Resolution
    HE Xi-Wen, CHEN Ding, WANG Yong-Tai
    1995, 16(6):  868-870. 
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    Based on the iterative target transformation factor analysis(ITTFA),a series of steps are taken to improve the component resolution function.These steps include the selection of an optimum set of wavenumbers and the selection of an optimum standard concentration matrix.This method can minimize the correlation of components obviously, so it is very useful to resolving the systems which are composed of spectra overlapped components.Three component system of o,m,p-chlorotoluene is presented in this paper.Satisfactory results are obtained.The influences of baseline correction and resolution on the calculated results are also discussed in detail.
    Studies on the Kinetic Behaviour of Cr(Ⅵ)in the Reaction Between Hydrogen Peroxide and Iodide
    ZHU Zhong-Liang, GU Zhi-Cheng, CHEN Rong-Mei
    1995, 16(6):  871-873. 
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    The Kinetic behaviour of Cr(Ⅵ)in the reaction between I-and H2O2in dilute H2SO4medium was investigated.It is found that Cr(Ⅵ)does not act as a catalyst of reaction between I-and H2O2but act directly as a oxidizing agent of I-.Amethod for calculating the reaction order is also proposed.It is unnecessary to know the concentration of reactant when this method is used.A Kinetic method for the simultaneous determination of Cr(Ⅵ)and Mo(Ⅵ)is proposed.The linear ranges of determination are 30～300 ng/mL for Cr(Ⅵ)and 2～20 ng/mL for Mo(Ⅵ),respectively.
    Synthesis of New Unsymmetrical Bisarylazoderivatives of Chromotropic Acid and Effect of Their Structure on Colour Reaction with Rare Earth,Thorium and Bismuth
    ZHANG Hua-Shan, ZHANG Jun-Feng, LI Xin-Yi
    1995, 16(6):  874-876. 
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    Eight unsymmetrical bisarylazoderivatives of chromotropic acid such as 2, 6-dichloro(bromo)chlorophosphonazo, 2, 6-dichloro(bromo)arsenazo and so on have been synthesized.The dissociation equillibrium of new chromogenic reagents have been investigated and their dissociation constants have been determined.These chromogenic reagents are applied to the determined rare earths,thorium and bismuth.
    Theoretical Study on Secondary Bond in Organo-Metallic Compound(I)──The Conjugated Bond and Secondary Bond in β-Chlorovinyl Mercury Chloride
    LAI Cheng-Ming, YUAN Man-Xue, TANG Jun, CUI Chong-Wei, LUO Xin-Cai
    1995, 16(6):  877-880. 
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    According to the analysis of experimantal data, we found that:(l)crystal structure indicates that the title trans-molecule has a plane structure; (2)The vector sum of bond-moment of individual single, double and triple bond can not be used to explain the molecular dipole moment; (3)Raman spectrum misses characteristic frequency of vibration of double or triple bond; (4)Ultra-violet absorption λmaxshifts toward red; (5) C-Cl bond in chloroethylene molecule and C-Hg bonds in diphenyl mercury molecule are proved to be conjugated. Thus we infer there exists a conjugated bond Ⅱ56in the title molecule including the vacant 6pzorbital of mercury. In order to further study the formation of this conjugated bond,we applied MNDO semi-empirical molecular orbital calculation to these cis- and transmolecules.The results show that in each molecule, there exist some π molecular orbitals involving empty 6pzorbital of mercury atom, the C-Hg bond has about 0.1 π-bond order,thus it proves the vacant 6pzorbital of mercury indeed participates in the formation of conjugated system.By comparison of the difference of properties of cis- with trans- compound, we found that the cis- one has a higher melting poin,more negative heat of formation and the heat of elimination of C2H2from this molecule, less quantity in isotope exchange,its decompostion in alcohol is more slow, and its 1,4-reaction is more difficult to take place.In view of above distiction it shows that cis-molecule is more stable than trans-one. Thus we assumed that in cis-molecule there is a weak secondary chemical bond which located in the plane of molecule,essentially it is a weak three centers with four electrons delocalization bond. MNDO calculation supports this view point.In, in l964, the author already predicted the existence of this bond in abovemolecul.
    Studies on the Application of Lanthanoid Metalto Organic Reactions──The Reaction of Anhydrous NdCl3/Lithium Naphthalide System with Ketones or Isocyanates or Isothiocyanates
    BAO Jian-Chun, BEI Mei-Zhi
    1995, 16(6):  881-886. 
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    This paper reports the reactions of anhydrous NdCl3/LiNp(LiNp=Lithium Naphthalide)system with benzoplienone,α,β-unsaturated carbonyl compounds,isocyanates and isothiocyanates, respectively.It is found that the anhydrous NdCl3/LiNp system can promote a novel cyclodimerization of α,β-unsaturated carbony compound to give(IR*,2S*,3R*,4S*)-cyclopentanol derivatives and their stereoisomer.The same system can also react with isocyanates or isothiocyanates to give the corresponding reductive coupling products in good yield.We also found that the new system of NdCl3/LiNp/Ligand,which differs from the NdCl3/LiNp system, shows a different selectivity in the reaction with benzophenone to mainly give diphenyl methanol.
    Ansa-Metallocene Derivatives(Ⅰ)──Syntheses and Structures of Sila-bridged Bis(1-indenyl) and Tetrahydroindenyl Titanium Complexes
    ZHOU Xiu-Zhong, WANG Bai-Quan, XU Shan-Sheng
    1995, 16(6):  887-891. 
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    The chiral ansa-metallocene derivative sila-bridged bis(1-indenyl)titanium dichloride(Me2SiOSiMe2)[Ind]2TiCl2(1)has been prepared by the reaction of the dilithium salt of 1,3-bis(1-indenyl) tetramethyl disiloxane with TiCl4·2THF.After catalytic hydrogenation,1 has been converted to the corresponding tetrahydroindenyl complex (Me2SiOSiMe2)·[IndH4]2TiCl2(2).The crystal structures of 1 and 2 have been determined by X-ray diffraction analysis.Both the crystals belong to monolinic, space group P21/n.For 1,a=1.0546(4)nm,b=1.3773(7)nm,c=1. 5493(5) nm;β=99.05(3)°,V=2.222(1)nm3,Z=4,Dc=1.43 g/cm3,R=0.033.For 2, a=1.0911(2)nm,b=1.3815 (3)nm,c=1.5886(2)nm;β=101. 39 (1)°,V=2.347(1)nm3,Z=4,Dc=1.378g/m3,R=0.053.
    The Synthesis and Properties of N-(β-Ttiphenylgermalyl) propionyl-α-amino-methylphosphonates
    CHEN Ru-Yu, MAO Li-Juan
    1995, 16(6):  892-895. 
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    In this paper,two series of N-(β-triphenylgermanyl)propionyl-α-aminomethylphosphonates have been synthesized and both conditions and mechanism of the condensation reaction of sterically hindered α-aminomethylphosphonate with β-triphenylgermanyl propionic acid were studied. Preliminary bioassays indicate that the title compounds compared with corresponding α-amino-methylphosphonates have more significant antitumor and anti-TMV properties.
    Syntheses and Antitumor Activities of New Spin-labeled 5-Fluorouracil Derivatives(Ⅲ)
    WANG Yan-Guang, CHEN Yao-Zu, XIAO Xin-Liang, LIU Rui-Xian
    1995, 16(6):  896-899. 
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    Nine new spin-labeled derivatives of 5-fluorouracil,2,5a-cand 7a-c,were synthesized and their structures were confirmed by IR,UV,MS and ESR spectra as well as elementary analysis.The antitumor activities of compounds 2 and 5a-ewere tested against S180 and EAC in mice.The preliminary results showed that the antitumor activities of compound 5ewas similar to that of 5-fluorouracil, while the acute toxicity of 5c(LD50=944.8my/kg)was about 8 times lower than that of 5-fluorouracil(LD50=117.2mg/kg).
    Studies on Synthesis and Biological Activities of N-Silylmethyl-N-formyl Aniline Derivatives
    ZHANG Zeng-You, SHANG Jian, ZHOU Xiu-Zhong
    1995, 16(6):  900-904. 
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    In the presence of the reaction of chloromethylsilanes with substituted anilines in DMF was studied. By means of elementary analysis,IR and 1HNMR,the products of these reaction are confirmed to be N-silylmethyl-N-formyl aniline derivatives.Twenty-three new compounds(with the general formula:RR'R″SiCH2N·where R=CH3;R'=CH3,p-ClC6H4;R″=p-ClC6H4,p-FC6H4,C6H5;Xand Yare H,CH3,Cl,Frespectively.)have been synthesized.The biological activities of some compounds have been tested,a few of them have good germicidal activities.thus p-FC6H4Si(Me2)CH2N(CHO)C6H4Cl-p at 0.005% gave 100% control of Asparagus stem blight.
    Synthesis and Characterization of Phthaloyl Bridged Iron-Sulfur Complexes [(μ-RS)Fe2(CO)6]2(μ-OCC6H4CO-μ)
    SONG Li-Cheng, HU Qing-Mei, SU Zheng-Yuan, CAO Xi-Chuan, ZHU Jin
    1995, 16(6):  905-908. 
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    The in situ reaction of the complex salts [(μ-CO)(μ-RS)Fe2(CO)6]Et3NH derived from Fe3(CO)12,RSH and Et3N with p-,or m-phthaloyl chloride in THFat room temperature afforded six novel phthaloyl bridged iron-sulfur complexes [(μ-RS)Fe2(CO)6]2(μ-pOCC6H4CO-p-μ)(R=Et,n-Bu, t-Bu) and [(μ-RS)Fe2(CO)6]2(μ-m-OCC6H4CO-m-μ)(R=n-Pr,n-Bu,t-Bu).These new complexes were characterized by elemental analysis,IR and 1HNMR spectroscopies and the reaction course was discussed.In addition,a new synthetic route to p-phthaloyl chloride has been developed.
    Studies on the Biomimetic Oxidation Catalyzed by the Model Compound of Cytochrome P-450(Ⅴ)──The Influence of Substituent R in T(R-T)PFe(Ⅲ)Cl on the Monooxygenation of Cyclohexane
    JIAN Du-Xiao, GU Chen, GUI Ming-De, ZHU Shen-Jie
    1995, 16(6):  909-912. 
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    The influences of monosubstitution at phenyl rings in a series of T(R-P)PFe(Ⅲ)Cl(R=o,m,p-Me,MeO,Cl,Br,I,NO2, o-t-Bu,p-t-Bu,o-NH2,Et,i-Pr)on the biomimetic catalytic monooxygenation of cyclohexane with PhIO were studied.The yields of cyclohexanol were increased by the electron-with drawing substituents Rin these catalysts T(R-I)PFe(Ⅲ)Cl.Afair linear correlation between the yield of cyclohexanol and para substituent constant σpis presented as:lgYR/YH=3. 2σp-0. 03. The steric effect of all ortho substituents in T(R-P)PFe(Ⅲ)Cl increased the yield of cyclohexanol sufficiently.
    Studies on the Total Synthesis of Taxamairin B
    WANG Xue-Chao, ZHANG Chi, PAN Xin-Fu, CHEN Yao-Zu
    1995, 16(6):  913-914. 
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    Taxamairin B,a novel rearranged 9(10→20)-abeo-8,11,13-triene diterpene,containing a tropone ring system has been synthesized from commercially available catechol and 1,3-cyclohexandione by a short and efficient route.A Friedel-Crafts annunation and the oxidation of the allylic and benzylic methylene group are the key steps.
    Synthesis of Ribozyme Substrates Containing Chiral Methylphosphonate at Cleavage Site
    ZHOU Ying-Zi, WANG Lai-Xin, ZHANG Li-He
    1995, 16(6):  915-916. 
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    Two stereoisomers of dicytidylyl methylphosphonate 10 and 11 were synthesized and used as a block for the synthesis of ribozyme substrates containing chiral center at the cleavage site.
    Sulfonation of Deactivated Benzene Derivatives
    ZOU You-Si, DAI Li-Zong, LIN Jing
    1995, 16(6):  917-919. 
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    The reactions of benzenesulfonic acid,diphenyl sulfone,nitrobenzene,benzaldehyde,benzoic acid, methyl benzoate and benzophenone with SO3using dichloromethane as the solvent at room temperature were studied by analysis of the resulting mixtures of the sulfonated derivatives with 1HNMR. The initial sulfonation of the benzene derivatives yields the corresponding 3-sulfonic acid.With the exception of nitrobenzene and methyl benzoate,small amounts of 3, 5-disulfonic acid,in addition, undergoes sulfonation giving 3,3-di and 3,5,3'-trisulfodiphenyl sulfone.
    N2-Binding Site in Nitrogenase and Ammonia Synthesis with Iron Catalysts
    HUANG Jin-Wei, ZHANG Feng-Zhang, XU Liang-Shu, ZHUANG Hong-Tu, WAN Hui-Lin, CAI Qi-Rui
    1995, 16(6):  920-923. 
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    Ethylene was used as a probe to detect the N2-binding site in nitrogenase.It was found that ethylene couldn't compete with N2 in the nitrogenase system.So the N2-binding site in nitrogenase might probably be the mode of 6Fe[μ6(η2,ε4)]and the mode of 3Fe +1Mo[μ4(η3,ε1)] in the cage of the protein-bonded FeMo-co, but not be the mode of dinuclear coordination occurred on the 2Fe-sites at the gap of FeMo-co.In ammonia synthesis with iron catalysts,the N2-binding site might probably be the mode of 6Fe [μ6(η3,ε3)].
    Microcalorimetry Applied to the Study of Catalase Reaction
    LIANG Yi, WANG Cun-Xin, WU Ding-Quan, SONG Zhao-Hua, QU Song-Sheng, ZOU Guo-Lin
    1995, 16(6):  924-928. 
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    Microcalorimetry and thermokinetic equations were used to study H2O2decomposition by beef liver catalase.The catalase reaction obeyed the Michaelis-Menten kinetics,and at 298.15 K and pH 7.0,the Michaelis constant (Km),the turnover number and the molar enthalpy(ΔrHm)of the reaction were 2.36×10-2mol/L,1.20×104s-1and -83.67 kJ·mol-1,respectively.The later period of catalase reaction was a first order reaction for H2O2,=6.31×105L·mol-1·s-1and k1=6.31×10-5/[Eo]s-1,respectively.The catalase reaction obeyed Ogura mechanism,and the ternary complex decomposition rate constant was 6.00×103s-1.
    Studies on Oxydehydrogenation of Ethane to Ethene on Li+/MgO Catalysts(Ⅲ)─The Mechanism of Catalytic Action
    CAI Bing-Xin, ZHENG Xiao-Ming
    1995, 16(6):  929-932. 
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    The oxydehydrogenation of ethane to ethene has been studied over Li+doped with MgO catalysts with various Li+contents. In this paper,we investigated the catalytic mechanism of oxydehydrogenation on Li+/MgO with XRD,IR,TG.It is found that the quantity of Li+doped with MgO affect amounts and intensity of acid and basic centres, surface metal ions and oxygen groups with low coordination are active species for the reaction.The oxydehydrogenation of ethane to ethane on Li+/MgO is probable by the simultaneous action of radical and ionic mechanism.
    ESR Study of Superhyperfine Interaction of 127I in[Cu(IO5OH)2]5-Ion Complex
    ZHAN Rui-Yun, XU Jie, LIU Gui-Zhen, LIU Ya-Yan, WU Ming-Mei, SU Qiang, SONG Rui-Fang
    1995, 16(6):  933-936. 
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    ESR method has been used to study superhyperfine interaction of 127I in [Cu (IO5OH)2]5-ion for Na4KCu(IO5OH)2·12H2O single crystal.The main purpose of this paper is to confirm the existence of unpaired electron spin on iodine atom and to find a reasonable explanation for the spin delocalization of Cu2+ions. Based on the ESR parameters of paramagnetic [Cu(IO5OH)2]5-ions,the calculated results show that about 0.77% of the unpaired eletron spin is located on each iodine atom.
    The Effect of Cationic,Anionic and Nonionic Surfactant Micelles on the Alkaline Hydrolysis of Esters
    ZENG xian-Cheng, LI Qi-Lin, QIN Zi-Ming, WANG Qian, ZOU Ping, LI Gan-Zuo, HUANG Qi-Zhong
    1995, 16(6):  937-942. 
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    The alkaline hydrolysis of aromatic and normal aliphatic acid esters has been studied at 25℃ in the micellar solutions of surfactants(DTAB,TTAB,CTAB,SDS,Brij-35,Triton X-100) with spectrophotometry and the method of thermokinetics in this paper.k1mand k2min micellar pseudophase have been calculated.The ratios of k2mto k2wor k1mto k1windicate that the alkaline hydrolysis of esters are inhibited by all researched micelles.We suppose the micropolarity of micelles can account for the inhbition of micelles.
    Effect of Acid Treatment on the Structure and Acidity of Beta Zeolite
    SHEN Jian-Ping, LI Yue, SUN Tie, GUO Jun, ZHANG Bo, JIANG Da-Zhen, MIN En-Ze, JIANG Ting-Shun
    1995, 16(6):  943-947. 
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    The effect of acid treatment on the structure and acidity of β zeolite was investigated. It was found that βzeoliteis easily dealuminated by acid treatment,but it can resist 5 mol/L HCl solution.The degree of dealumination is higher than 80% in the 5 mol/L HCl solution.In the acid solution the stability of polymorph(A)is less than that of(B).The chiral of βzeolite can be modified by acid treatment.The results of adsorption, NH3-TPD and pyridine-IR show that the pore volume does not change obviously,the acid strength of sample changes with acid treatment and reaches its maximum in the sample with the Si/Al of 38.8.Lacid is the main acid sites on the surface and increases with increasing the value of Si/Al ratio.
    Preparation of Carbon Nanotubes from Laser Ablation
    CHENG Da-Dian, YU Rong-Qing, LIU Zhao-Yang, ZHANG Qiang, WANG Yu-Huang, HUANG Rong-Bin, ZHAN Meng-Xiong, ZHENG Lan-Sun
    1995, 16(6):  948-949. 
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    Carbon nanotubes were prepared by laser ablating the graphite drown in the water and characterized by transmission electronic microscope.In addition to the nanotubes,spherical carbon balls with diameters as large as one micrometer were observed as the products from laser ablation.
    Preparation of Fine Powders within the Pore of Active Carbon
    ZHAO Zhen-Guo, CHENG Hu-Min, MA Ji-Ming, QI Li-Min
    1995, 16(6):  950-951. 
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    Anovel method of synthesizing PbTiO3powders within the pore structure of active carbon from a solution containing PbAc2 and Ti(OBu)4with 1:1 molar ratio has been investigated.X-ray diffraction indicated that the calcined powders at 600℃ showed characteristic peaks corresponding to tetragonal PbTiO3Due to the compartmentalizing effect of the pore structrue of active carbon,fine PbTiO3powders with nanometer size can be prepared by the method.
    Establishment of New Research System to Combine Electrochemistry and Electron Spectroscopy and the Investigations of Surface Chemical States of Pt/BiadElectrode
    SUN Shi-Gang, CHEN Sheng-pei, CHEN Bao-Zhu, XU Fu-Chun, XUE Guo-Qing, LIN Wen-Feng, GE Fu-Yun
    1995, 16(6):  952-954. 
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    A new research system,which allows samples to be transferred rapidly and without contamination between electrochemical environment and ultra-hight-vacuum chamber,has been set up recently. This system is of interest to combine investigations on structure and proporties of solid surface at both solid/liquid and solid/gas interfaces.The prelimiary study of Pt/Biadelectrode at levels of chemical environment and electronic structure demonstrated the success of the system established.The XPS data indicate that two oxidation states of Bi adatom existe on Pt/Biadelectrode surface.The present results give new interpretation of the promoting mechanism of Bi adatom in electrocatalysis.
    Reduction of Carbon Dioxide to Carbon with Active Cation-Excess Magnetite
    ZHANG Chun-Lei, WU Tong-Hao, YANG Hong-Mao, JIANG Yu-Zi, PENG Shao-Yi
    1995, 16(6):  955-957. 
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    The cation-deficient magnetite(Fe3+δO4,δ<0)was synthesized by the oxidation of Fe(OH)2suspensions at 358 K.The cation-excess magnetite(Fe3+δO4,δ>0)was obtained by flowing H2gas through magnetite with cation-deficient composition at 563 K.The stability of Fe3+δO4(δ>0)was investigated at various temperatures and atmosphere.The reactivty of Fe3+δO4(δ>0)of reducing CO2gas into carbon was studied at 358 K.The results confirm that CO2was nearly 100% decomposed into carbon,the oxygen in CO2is transferred in the form of O2-to the cation excess magnetite.The bigger the cation-excess extent of magnetite,the higher the decomposability of CO2,and the more O2is produced indirectly.
    Preparation of Molecular Deposition Film of Bacteriorhodopisin
    LI Zheng-Qiang, WANG Li-Yan, ZHANG Xi, LI Bo-Fu, SHEN Jia-Cong, HU Kun-Sheng, WANG Ao-Jin
    1995, 16(6):  958-960. 
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    The molecular deposition (MD) film of Bacteriorhodopsin was prepared for the first time.UV-Vis spectra were used to follow the deposition process and a uniform growth process of the MDfilm was proved.We also observed larger BRmolecule gathering body of single layer MD film.Raman spectrum shows that the combination of BR with PyC6BPC6Py does not affect the structure of BR.
    Studies on Semiconductor Properties of CMD and Its Activity in the Alkali Battery
    ZHANG Bi-Quan, LU Zhao-Zhong
    1995, 16(6):  961-963. 
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    CMD sample was made by direction oxidive method following the densification.The diffusion of proton in MnO2affects the electrochemical activity in the alkali battery.The results show the CMD reveals the characteristics of n-type semiconductor.The concentration and transference of proton in CMD after densification are increased.The wide diffusion way for proton is important to improve the discharge behavior of CMD in 9 mol/L KOH.
    Studies on the Ground and Excited States of NH2by SAC-CI and Topological Method
    ZHENG Shi-Jun, CAI Xin-Hua, SONG Tian-Le, MENG Ling-Peng, H. Nakatsuji, M. Hada
    1995, 16(6):  964-966. 
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    The ground state(2B1)and excited states (2A1,2B2) of NH2were investigated by SAC-CI method. The potential surface of the second excited state (2B2) and the equilibrium geometry of tl1is state were obtained.The topological properties of density super-surface of the states were discussed,from which the bond angle increasing and decreasing as the excitation form ground state to excited states (2A1, 2B2) were discussed also. Having a ▽ type bond structure,the dissociation of the equilibrium geometry of (2B2) state should be as the way of separation of H2 and N.
    Synthesis of Two New Hydrogen Bond Induced Liquid Crystals
    TIAN Yan-Qing, LIN Feng, ZHAO Ying-Ying, LUO Xu-Yang, TANG Xin-Yi, SU Feng-Yu, ZHAO Xiao-Guang, ZHOU En-Le
    1995, 16(6):  967-970. 
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    Two new hydrogen bond induced liquid crystals with 4-butoxy benzoic acid as the proton donor and two chiral substituted stilbazole as the proton acceptor have been synthesized.Their liquid crystal transitions were studied by DSC and optical polarized microscope,the IRspectra of the complexes show the existence of the intermolecular hydrogen bond.The results of DSC and optical polarized microscope show that one of them(4BA-VSZ)has a chiral smectic Cphase.
    A Study of Ring-Opening Copolymerization of DL-Lactide and 2-Hydro-2-oxo-1,3,2-dioxaphosphorinane
    FAN Chang-Lie, LI Bing, LIU Zheng-Hua, ZHUO Ren-Xi
    1995, 16(6):  971-973. 
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    A new kind of water-soluble copolymers were prepared by ring-opening copolymerization of DL-lactide and 2-hydro-2-oxo-1,3,2-dioxaphosphorinane,using triisobutylaluminium as the initiator. The final copolymers were characterized by 1HNMR,IR spectrometry.The influences of the amounts of initiator and molar ratio of the monomers on the total conversion,monomer conversion,copolymer composition,intrinsic viscosity of the copolymers were investigated,respectively.
    Selective Anionic Polymerization of 2,3-Epoxypropyl Methacrylate
    HOU Yuan-Xue, ZHANG Hong-Min
    1995, 16(6):  974-977. 
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    The double bond selective anionic polymerization of 2, 3-epoxy propyl methacrylate has been carried out.It is found that the dominant by-reaction occurred in initiation process at lower temperature(<-40℃),not in propagating period,because of the interaction between initiator and epoxy group of monomer.This by-reaction can be restricted by the use of initiator with lower reactivity.On the other hand,higher polymerization temperature(>-20℃)will result in the cross-linking reaction, so it is difficult to control the double bond selective polymerization.GPC.1HNMR and FTIR measurements indicate that a soluble functional polymer with an epoxy group in each repeating unit and monodispersity (Mw/Mn<1.10) has been prepared by proceeding the polymerization with 1,1'-diphenylhexyllithium in THF at lower temperature.
    Studies on Selective Separation of Ethanol by Pervaporation Through Poly(vinyl alcohol)/Chitosan Blend Membrane
    WANG Xin-Ping, SHEN Zhi-Quan, ZHANG Fu-Yao, LIN Rong-Xuan
    1995, 16(6):  978-980. 
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    It has been recognized generally that glassy polymer membranes preferentially permeate water and elastomer membranes preferentially permeate ethanol.Until now only a few alcohol-selective membranes have been developed such as silicone rubber membrane,having low flux and selectivity toward alcohol.In this paper,preferential separation of ethanol from aqueous solution through hydrophilic PVA/CS blend membrane has been investigated for the t time.The results show that PVA/CS membrane preferentially permeate ethanol at lower ethanol concentration in feed,and the selectivity of chitosan membrane toward alcohol can be greatly improved by introducing water-soluble polymer PVAinto chitosan. The membrane with PVAcontent of 53% (wt%) gives a separation factor 17.1 and a flux of 217 g·m-2·h-1at 8.7%(wt%) of ethanol in the feed at 20℃. The separation properties of this membrane were much higher than those of silicone rubber membrane usually used as alcohol-selective one.
    Studies on Oriented and Unoriented Films of Liquid Crystalline Wholly Aromatic Copolyester B─N Using Technique of Banded Texture Decoration
    DONG Yan-Ming
    1995, 16(6):  981-983. 
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    Banded texture was decorated on oriented films of thermotropic aromatic copolyester B─N by annealing.The fibrils of three levels,which were macrofibrils of several ten mircron in diameter,fibrils of few micron and microfibrils of about 0.3 μm,were observed by using polarized microscope.After annealing,fibrils in different levels relaxed to different morphology.Macrofibrils still oriented along shear direction,but fibrils relaxed to be helical,and microfibrils relaxed to be waveform therefore the banded texture can be seen.On the other hand,both banded texture and fibrils decorated the annealed unoriented films,that revealed the distribution of directors within and out of domains and the variation of directors on boundaries.
    Selective Catalytic Hydrogenation of C=C in Poly (butadiene-co-acrylonitrile)Copolymer
    ZHANG Bang-Hua, WANG Guang, ZHOU Qing-Ye, HAO Guang-Jie, SONG Mou-Dao, ZHANG Ying
    1995, 16(6):  984-985. 
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    This paper studies the catalytic hydrogenation of C=C in poly(butadiene-coacrylonitrile) copolymers containing different amount of butadiene by using RHCl·[P(C6H5)3]3as the catalyst.The results of IR and NMR demonstrate that RhCl[P(C6H5)3]3is an efficient catalyst and shows an excellent selectivity.The catalyst provides quantitative hydrogenation of C=C unsaturation without any hydrogenation of CN.It is necessary to keep enough reaction time so that the double bonds can be hydrogenated completely.
    Synthesis and Structure Study of Hard-Segment Model Compounds in Poly(urethane urea)Block Copolymers
    LUO Ning, WANG De-Ning, YING Sheng-Kang
    1995, 16(6):  986-988. 
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    A series of hard-segment model compounds based on 3,5-diethyltoluene diamine,4,4'-diphenylmethane diisocyanate and phenyl isocyanate has been synthesized in this paper.The model compounds are microcrystals.Combined with WAXD analysis,the assignment of the bands at 1643 cm-1and 3290 cm-1in the FTIR spectra of the model compounds is given.Both bands are the hydrogen-bonded urea carbonyl and urea NH groups with the form of planarly bifurcated hydrogen bonds in the microcrystals,respectively.Melting points of the model compounds are almost the same as the change of average degree of polymerization by DSC experiments.
    Studies on New Type of Vinyl Acetate/Divinylbenzene Copolymers(Ⅱ)──Preparation,Structure and Properties of Saponified Copolymers
    WU Xiang-Dong, GUO Xain-Quan, HE Bing-Lin
    1995, 16(6):  989-991. 
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    The polymers possessing hydroxyl groups were synthesized by saponifying the copolymers of vinyl acetate and divinylbenzene.The effect of different degree of crosslinking on the saponification was investigated.The parameters of pore structures and swelling properties of these saponified copolymers were determined.The adsorption of aromatic amino acids to the saponified copolymers was studied.
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