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    24 October 1989, Volume 10 Issue 10
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    Articles
    Studies on the Polymerization of Aluminosilicate
    Li Shougui, Li Xikai, Xu Ruren
    1989, 10(10):  977-980. 
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    This paper describes a study of polymerization of aluminosilicate.The state and change of silicate and aluminate in starting materials and reaction mixture have been studied by using NMRtechniques, Laser-Raman spectroscopy and silicatemolybate method.It was found that the reaction between aluminate and silicate is very fast and silieate itself is degraded.Therefore, the process of further polymerization of aluminosilicate is the polymerization of low molecular species of aluminosilicate or silicate.It can be explained by using this point of view that the rate of polymerization of aluminosilicate is changed with variation of concentration of reagents.
    Studies on White Powdery Tungstic Acid (XVI)——Preparation and Properties of Dimethyl Sulfoxide Coordinated Muttivalent Metal Hexatungstates
    Zhu Sisan, Gu Yidong
    1989, 10(10):  981-984. 
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    The title compounds have been successfully prepared by the reaction of the respective metallic carbonates,acetates,nitrates or sulfates with dimethyl sulfoxide solution of white powdery tungstic acid.All these compounds are hexa- or deca- DMSOcoordinated hexatungstates, existed as well defined crystals,[(DMSO)6M(Ⅱ)][W6O19](M=Mn,Cu,Co,Ni,Zn,Ca)and[(DMSO)10M(Ⅱ)]2·[W6O19]3(M=Pr,Nd).The results of elemental analyses,IRand UVspectra are hereby preseted.The electro-chemical reduction behavior has also been studied.
    Studies on a New Tailed Porphyrinmanganese——The Reaction of a Tailed Porphyrinmanganese(Ⅲ)Complex wtth a Series of Organic Bases
    Shi Tongshun, Chi Xianglan, Wang Qingmin, Cao Xizhang
    1989, 10(10):  985-989. 
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    The reactions of a new tailed porphrinmangaanese complex, meso-mono-[o- (4-diethy-lamino)butyramidophenyl]triphenylporphyrin manganese (Ⅲ) chloride, PMn (Ⅲ)Cl, with organic bases were studied and the equilibrium constants of the axial addition reactions for these bases to PMn(Ⅲ)Cl in benzene were measured by spectral technique.Experimental results demonstrated that the reaction of this PMn(Ⅲ)l with aliphatic amines is a redox reaction,with pyridine is an incomplete redox reaction, and with imidazole is an axial addition reaction, respectively.The factors affected these reactions were also studied.
    Simultaneously Determining M ulticomponent of Acetaminophen Compound Tablets by Application of Partial Least Squares Method
    Wang Yiming, Luo Guoan, Wang Zhenpu, Zhou Guohua
    1989, 10(10):  990-993. 
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    The basic principle and computing method of the partial least squares method (PLS) applied to a multicompoent analysis were discussed.The optimum experimental condition of simultaneous UV-spectrophotometric determination of the contents of acetaminophen, aspirin and caffeine in acetaminophen compound tablets and the application of PLSin simultaneous multicomponent determination were studied.The average recovery ratio of the three components are 99.88±0.33%, 99.99± 0.14% and 99.92±1.24% (confidence 95%), respectively.No information has ever been available in the literature for the application of PLSto the pharmaceutical analysis.
    On-line Simultaneous Determination of Mixtures by UV Spectrophotometryand Kalman Filter
    Shi Leming, Zhang Maosen, Liu Xinan, Lin Aihua, Jia Zunsheng
    1989, 10(10):  994-998. 
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    This paper describes the simultaneous determination of mixtures by UV Spectrophotometry and Kalman filter based on the IBM PC/AT-DMS200 UV/vis on-line system.Satisfactory results were obtained for the analysis of synthetic and waste water samples of two different mixture systems by the proposed method.
    Making and Characteristics of a PVA Immobilized Urease Electrode
    Chen Peiqin, Xie Weiwen, Lin Sicong
    1989, 10(10):  999-1001. 
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    Aurease electrode immobilized with polyvinyl alcohol hydrogel (PVA) was made and its response characteristics were studied under different concentrations of urea (Curea) and at different temperatures and in a buffer solutiont with different pHvalues.It is revealed that for this kind of urease electrode the highest response speed is at 30℃ and pH 9.3, and the maximum steady state potential is at 33℃ ; meanwhile, there exist linear relationships of both v～lg Curea and E～lg Curea in the urea concentration ranges of 3.4× 10-4～2.0× 10-2 mol·L-1 and 2.0×10-4～3.7×10-2 mol·L-1, respectively.
    Study of Caged Bicyclic Phosphates (Ⅱ)——Synthesis of Derivatives of 1-Sulfo-1-Phospha-4-Methylene-2,6,7-Trioxabicyclo[2,2,2]octane
    Li Yugui, Wang Jianji, Liu Yunshan, Han Jiaxiang, Cao Jinhong, Jiang Xiaochun
    1989, 10(10):  1002-1006. 
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    Eleven new compounds with the formula 3 were synthesized by phosphonothiolation reaction of bicyclic phosphate 1 with phosphonothioyl chloide 2 in the presence of DMAP(4-N,N-dimethy-laminopyridine) and Et3N.The outstanding catalysis of DMAPis studied.The structure of compound 3 was confirmed by elemental analysis, IR, 1H NMRand MS.It has been shown that some of these compounds have activities of plant growth regulator by the priliminary biological tests.
    Studies on the Synthesis and Antitumor Activity of 3-Aminopropylsilatrane Derivatives
    Ding Qizhu, Luo Xuangan, Zhuo Renxi
    1989, 10(10):  1007-1011. 
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    Fourteen new derivatives of 3-aminopropylsilatrane were synthesized by the reaction of 3-aminopropylsilatrane with acids or 3-chloropropylsilatrane with amines.The structures of these compounds were identified with 1H NMR, IRand elemental analysis.The results of in vitro cell culture testing showed that some of the silatrane derivatives exhibit good antitumor activity.
    Research on Synthesis and Light Character of Two Kinds of Heterocyclic Pentadienes Containing Oxygen and Nitrogen
    Pan Jiaxing, Chen Jingshan, Kao Chenheng
    1989, 10(10):  1012-1016. 
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    p-(2-Phenyl-1,3,4-oxadiazol-5-yl)-4-(2'-phenyl-oxazol-5-yl)benzene and p-(2-phenyl-1,3,4-oxadiazol-5-yl)-4-(5' -phenyl-oxazol-2' -yl)benzene and ten of their derivatives are prepared.They are all new compounds.The UV, FL, IRspectra, laser conversion efficiency are detmermined.
    Synthesis of the Precursor of Acyloin Derivatives of Ferrocene——2-Ferrocenyl-2-(Aryl Hydroxymethyl)-1,3-Dithiane
    Sun Lijun, Shi Shujian
    1989, 10(10):  1017-1021. 
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    The aim of this work is to develop a new route for the synthesis of ferrocenyl acyloin derivatives.The route consists of the reaction of 2-ferrocenyl- 1, 3-dithiane with aryl carbonyl compounds to form a class of intermediates, 2-ferrocenyl- 2- (aryl hydroxylmethyl)-l,3-dithianes(Ⅲ), which are then hydrolyzed to afford the desired products.In this paper we only report the synthesis and some properties of the intermediates (Ⅲ).Sixteen of the intermediates (Ⅲ) are obtained, they are all new ferrocene derivatives.
    The Electrochemical Catalysis Behavior of Metal-Porphyrins for Thionyl Chloride Reduction
    Li Changming, Zha Quanxing, Yang Lin, Li Xiang
    1989, 10(10):  1022-1025. 
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    The electrochemical catalysis behavior of thionyl chloride reduction with metal- tetram-ethoxyphenyl porphyrins is studied.The experimental results demonstrate that metal porphyrins possess a higher activity for thionyl chloride reduction and the order of the activity of porphyrins with different central ions is Fe≈Co>Ni.In the other hand, these complexes seem to retard the deposition of LiCl on the electrode surface and to inhance the discharge capacity of Li/SOCl2 batteries.
    Electrochemical Study of (RC2R')Co2(CO)6 and Their Reaction with Lewis Base
    Meng Qingjin, Sun Shouheng, Bu Xiuren, You Xiaozeng
    1989, 10(10):  1026-1029. 
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    Two new clusters (C6H5C2C6H4-Br-p)Co2(CO)6-n(PPh3)n(n= 1,2) were synthesized.The electrochemical behavior of a series of (RC2R')Co2(CO)6-nLn(n=0,1,2;L = PPh3) and (RC2R').Co2(CO)6 in the presence of PPh3were studied in acetone by utilizing cyclic voltammetry.For (RC2R')Co2(CO)6-nLn, their main electrode processes are as follows:(RC2R')Co2(CO)6-n, Ln+e=(RC2R')Co2(CO)6-n, Ln-The reduction potential of this process is related to both RC2R' and L.The larger the charg density in C2Co2, the more difficultly by the cluster is to be reduced and the easier to be oxidized, which indicates that the energy level of frontier molecular orbital of cluster is related to both cobalt and ligand.The cluster radical is a catalyst for electron transferred catalyzed (ETC) reaction.
    Kinetic Study of Axial Coordination of Para-Substituted (Tetraphenylporphinato) Iron(Ⅲ) Chloride
    Zhu Zhi'ang, Ma Yuxin, Chen Rongti
    1989, 10(10):  1030-1035. 
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    Akinetic study is reported for the axial coordination of imidazole(Im).with para-substituted (tetraphenylporphinato)-iron(Ⅲ) chloride [Fe(p-X)TPPCl; X=Cl, H, CH3, OCH3] in acetone by means of Union Giken RA-401 stopped-folw spectrophotometer.The mechanism is postulated as follows:(这里有图片19891013-1030-1.gif)The experimental data were treated with CA-033Emicro computer.The equilibrium constant (K) of the preequilibrium step(l) and the rate constant(k) of the rate determining step(2) were obtained.The standard enthalpy △H?and standard entropy △S?of step (1), and the activation parameters △Hand △S≠of step (2) were calculated.It was found that linear relationships exists between the following pairs : △H?and the Hammett constant δ; △S?and δ ; △H≠and δ ; △S≠and δ; lnKand δ; lnk and δ.The isokinetic relationship between △H≠and △S≠was also found.
    Statistical Characterization on the Molecular Chain Structure of Ternary Multi-Block Copolymers
    Li Min, Zhang Chunshan, Chen Xinfang, Tang Aoqing
    1989, 10(10):  1036-1041. 
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    In this paper, by using the generating function method, the expressions of the average molecular weight and the molecular weight distributions of ternary multi- block copolymers of type are derived, giving a theoretical method for characterizating the molecular structure of this block copolymer.The properties of some block copolymers composed of the prepoly-mers with a special molecular weight distribution are discussed.
    Studies on Synthetic Bilayer Membranes (Ⅱ)——Synthesis of HBBTAB and Self-Organizing Behavior of the Amphiphile in Dilute Aqueous Solution
    Li Gouwen, Wang Zhiqiang, Tian Yongchi, Liang Yingqiu
    1989, 10(10):  1042-1043. 
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    Anovel single-chain amphiphile with the biphenyl moiety and the hexadecyl tail as the hy-drophobic group has been synthesized.The product was confirmed by elemental analysis,IRand 1H NMR.The self-organizing behavior and aggregate vesicles in dilute aqueous solution of the amphiphile were examined by electron microscopy.This indicates that the titled amphiphile is of practical bilayer -forming, capable of organizing biomembrane used as a mimetic agent.The 1H NMRspectra suggest that the molecular movement of the amphiphile was highly restricted within the aggregate.The gel-to-liquid crystal transition of the bilayer was shown by differential scanning calorimetry(DSC).These results show that the vesicle structures are composed of the bilayer similar to that of biomembranes.
    Determination of Thermodynamic Parameters for Adduct Reaction of 1,3-Diphenyl-l,3-Propanedione Copper CuC30H22O4 withFuran and Thiophen by GL-Chromatographic Method
    Zhou Jingyu, Guo Boshu, Yao Yuangen, You Xiaozeng
    1989, 10(10):  1044-1046. 
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    Using the GLCmethod, soluble equilibrium constant KR0 of Lewis bases furan C4H4Oand thiophen C4H4Sin the dibenzyl diphenyl solvent, and the apparent equilibrium constant KRfor the interaction between the two Lewis bases and the Lewis acid transition metal complex 1,3-diphenyl-1,3-propanedione copper at various temperatures are determined.
    Studies on the Complex of Actinide Elements with Crown Ether (Ⅲ)——The Crystal Structure of [UO2(NO3)2(H,O]·(B15C5)
    Wang Xin, Zhu Yin, Gan Xinmin, Tang Ning, Tan Minyu
    1989, 10(10):  1047-1049. 
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    The title complex crystallizes in triclinic, space group P1 with Z = 2.Lattice parameters are:a=8.468(2),b=8.787(2),c=16.674(4)Å,α=74.91(4)°,β=82.45(3)°,γ=69.84 (2)°, V=1123.4 Å3.The structure was solved by Patterson and Fourier techniques and refined by full-matrix least-squares to R=0.032 based on 4300 observed reflections.The linear uranyl group is perpendicular to a equatorial plane formed by six oxygen atoms, of which two from two water molecules, four from two bidentate nitrate groups.The coordination polyhedron takes a slight distored hexagonal bipyramid arrangement.The neutral UO2(NO3)2(H2O)2 units connect with crown ether by hydrogen bonding through intermediary water molecules.
    Investigation on Polarography with Linearly Changing Potential (X)——Oxidation of Dihydronicotinamide Adenine Oinucleotide at a Glassy Carbon Electrode
    Zhong Wenying, Zhang Jianrong, Zhang Zuxun
    1989, 10(10):  1050-1052. 
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    Oxidation of dihydronicotinamide adenine dinucleotide(NADH) at a glassy carbon electrode is investigated in this paper.The oxidation of NADHis a totally irreversible reaction with single electron and obeys the peak current equation for a totally irreversible wave after the electrode surface has been pretreated and washed electrochemically.The diffusion coefficient, transfer coefficient and the rate constants were determined,and the mechanism of oxidation of NADHis also discussed.
    A Study on the Indexing of X-Ray Diffraction Values of Powder Crystal Specimens for 2-Nitro-4-Methylphenylarsonic Acid
    Han Jiancheng, Zhu Xiaolei, Wu Xinran
    1989, 10(10):  1053-1055. 
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    The X-ray diffraction values of powder crystal specimens of unknown crystal system of 2-nitro-4-methylphenylarsonic acid were indexed successfully by the improved trial-and-error method.This method is also suitable for indexing for powder diffraction values of hexagonal, tetragonal, or-thorhombic, monoclinic and triclinic substance.The lattice parameters obtained from the powder diffraction values were refined by the least-square method.Indexing of the powder diffraction data and refinement of the unit-cell parameters for 2-nitro-4-methylphenylarsonic acid are reported.The refined crystallographic data are:C7H8NO5As, 10-C2h1-P2/m(approximately).a= 10.466(8)Å, b = 8.389(2)Å, c=9.918(3)Å, β=95.08(3)°, Z=4, Dm=1.970, Dx= 1.999 g·cm-3.The quantitative figure of merit(FN) is F20=27.
    A Study of Kinetics for the Solvent Effects on the Reaction Between MoOS2(S2CNEt2)2 and PPh3
    He Hong, Yang Huixing, Hu Jiaoping
    1989, 10(10):  1056-1058. 
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    The reaction kinetics between MoOS2(S2CNEt2)2 and PPh3 was studied in various organic solvents with the aid of the stopped-flow technique.The linear relationships between the kinetic parameters, such as In k, activation energy E, and a function of dielectric constant of solvents (ε- 1)/ (2ε+1) were found.The reaction mechanism is also discussed in this paper.
    Theoretical Study on the Isomerization Reaction of Silene
    Ju Guanzhi, Ma Wanyong, Deng Conghao
    1989, 10(10):  1059-1061. 
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    The titled isomerization, H2SiCH2→HSiCH3, was studied at HF/3-21Glevel.The variations in thermodynamic functions and the rate constant for this reaction are calculated.Considering both the thermodynamic and kinetic factors, we think that this isomerization reaction is favourable at a higher temperature.This conclusion is agreed with the experimental result.There is no effect of methyl substitution.
    Determination of Si—H Contents in Polydimethylmethylhy-drosiloxanes by 29Si NMR
    Sun Jiazeng, Ye Hongwei, Hu Gengyuan, Hu Xingdi
    1989, 10(10):  1062-1064. 
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    The Si-Hcontents in the polydimethyimethylhydrosiloxanes were determined by 29Si NMR.When Si-Hcontents range from 0.1～1.29, the results of determination correspond to those determined by chemical method.
    Studies on Solution Properties of Polyepichlorohydrin
    Li Houqiang, Chen Deben, He Jianye, Huang Guanglin
    1989, 10(10):  1065-1067. 
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    This paper presented the fractionation of the amorphous polyepichlorohydrin sample with a high molecular weight by reprecipitation with toluene as the solvent and ethyalcohol as the precipitant (50℃).The intrinsic viscosities [η] of the narrow distribution fractions in the solvents cyclohexanone (35℃) and tetrahydrofuran (25℃) were determined, the average values of the constants of Huggins equation and kraemer equation were obtained by calculation as K' = 0.360,β=0.146(in THF) ; K' = 0.356,β=0.148 (in cyclohexanone).The weight-average molecular weight of the fractions were measured experimentally by the low angle laser light scattering (LALLS) photometer, and the Mark-Houwink equations were calibrated as [η]= 2.37 × 10-5Mw0.79(dL/g,THF, 25℃), [η]= 1.36 × 10-5Mw0.85 (dL/ g, cyclohexanone, 35℃).The unperturbed parameters of molecular chains of polyepichlorohydrin were obtained according to the stockmayer-Fixman equation, k0= 5.25 ×10-4 (dL/g),σ=l.57,C∞ = 4.91(THF,25℃);k0= 4.97× 10-4(dL/g), σ=l.54,C∞ = 4.73(cyclohexanone, 35 ℃).
    Studies on Initiation Mechanism of Persulfate-pyrrolidine System in Acrylamide Polymerization
    Guo Xinqiu, Qiu Kunyuan, Feng Xinde
    1989, 10(10):  1068-1070. 
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    Kinetic study of acrylamide (AAM) polymerization was carried out with persulfate-pyrroli-dine(PyD) system as the initiator and revealed that PyDis an accelerator for acrylamide polymerization.The initial free radicals of persulfate-PyDsystem was studied by spin trapping technique and ESRspectrum.The result confirms that the pyrrolidinyl free radical is one of the primary free radicals responsible for AAMpolymerization.
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