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    24 October 1986, Volume 7 Issue 10
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    Articles
    The Protonation Constants of Some Aminopolycarboxylic Acids and the Stability Constants of Their Calcium Chelates in the Medium Containing Bile Acids
    Ji Ji, Xu Shanjin, Wang Kui
    1986, 7(10):  865-870. 
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    For the determination of the protonation constants of aminocarboxylatc ligands and the stability constants of their calcium chelales in the presence of cholate and deoxycholate,some modifications were introduced into the traditional potcntiomet-ric method.Obviously,these constants,thus determined are in nature,conditional,because the bile acids are surfactants,acids as well as complexing agents.By means of these methods,the conespending constants for EDTA,DTPA,EGTAand NTAwere determined as the function of the concentration of bile acids.The bile acids affect both the proton transfer t.nd coirpkxation prcccsscs,but the protonation constants change less than the stability constants.It is noted that the bile acids affect these constants in some concentrations lower than CMC.Thus their oligomer bind with cations(H+or Ca2+).
    Complexs of Crown Ether with the Rare Earth Nitrates(XIV)—Studies on Solubilities of the Ternary System La(NO3)3·4H2O-B12C4-CH3CN at25℃
    Hang Haiying, Lu Yugang, Zhang Xifang, Wan Youjia
    1986, 7(10):  871-876. 
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    The solubilities of the ternary system La(NO3)3·4H2O-B12C4-CH3CNat 25℃ have been determined by the semimicro method in order to summarize general information of complexation about rare earth nitrates and crown ether B12C4 in organic solvents.The results indicate that there is only one complex La(NO3)3 B12C4·4H2Oformed,the possibility to form any other complcxs species with different stoichiometry has been ruled out.Arelatively stable complex species La(NO3)3·Bl2C4·2H2Owas synthesized.its characters were described by chemical analysis,I.R.spectra,U.V.spectra,spcctrophotometry,gas chromatogrpny,X-ray diffraction,themogravimetric and differential thermal analysis.
    Studies on Rare Earth Hydroboron Compounds (Ⅳ)—The Pyridine Oxide Complexes of Rare Earth(Ⅲ) Decahydrodecaborates
    Zhang Lun, Ding Zirong, Zhang Guomin
    1986, 7(10):  877-880. 
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    The pyridine oxide(PYO)complexes of rare earth(Ⅲ)decahydrodecabo-rates were prepared by the reactions between Ln2(B10H10)3nH2Oand PYOin ethanol medium.These complexes were characterized by elemental analysis,electro-conductance,IR,Raman,UVspectra,and TG-DTA They have the follow ing formulae [Ln(PYO)7]2(B10H10)3(Ln=Nd,Sm,Eu,Gd,Ho,Er,Tm,Yb).The PYOis boned to the rare earth via the oxygen atom.The molar conductance data indicate that these complexes are ionic and behave as 2:3 electro-tyles in water.These complexes are thermally stable and their thermal behavior were approached.
    The Study of Determination of Copper by Absorption Spectroelectrochemistry
    Huang Ganquan, Luo Huanguang, Chen Maobin
    1986, 7(10):  881-882. 
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    The interference effects of sodium,calcium,magnesium and aluminium on the determination of copper were examined.The results show that the presence of 5000ppm Na+,500ppm Ca2+,100 ppm Mg2+,in the analyte solution has no influence on the determination,the interference of aluminium on the copper is serious.The copper in corrosive and sodium chloride was determined directly.The results are satisfactory.
    Application of FAB-MS/MS to Structural Analysis of Saponins
    Chen Yaozu, Chen Nengyu, Li Haiquan, Zhao Fanzhi, Chen Ning
    1986, 7(10):  883-885. 
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    Atechnique of fast atom bombardment ionization in conjunction with colli-sional activation(FAB-MS/MS)has been successfully applied to structural analysis of saponins.FABmass spectra exhibited protonated or sodium adduct molecular ions,which may be used for unambiguous assingment of the molecular weights of the glycosides.The collisional activation spectra of the selected quasi-molecular ions(M+H)+gave a series of characteristic fragment ions promising to give a clear picture for defining the sequences of the constituent saccharide units of the glycosides and for identifying the glycone.The experimental results show that the MIKESspectra can also provide sequence information just as CAspectra do but the sensitivity of the former is much less than that of the latter.Compounds 1 and 2 are known compounds.The structural analysis results of these compounds by this technique are in agreement with that reported in the literature by conventional methods.Compounds 3 and 4 are two new compounds.
    The Synthesis of Meso-Tetrakis-(4-Acetyloxylphenyl) Porphine and the Spectrophotometric Study of Its Colour Reaction with Lead
    Wang Dongjin, Jin Changming, Chen Tianfu, Huang Zexing, He Shuqiong
    1986, 7(10):  886-888. 
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    The water-insoluble porphine,meso-tetrakis-(4-acetyloxylphenyl)porphine(T(4-AOP)P),has been synthesized and its colour reaction with lead(Ⅱ)has been studied.The lead(Ⅱ)complex was formed in the presence of sodium dode-cyl sulfate.The complex formation was slow at room temperature,however,it could be accelerated by heating at 100℃ for 12 min.The soret band of the complex lies at 466nm,which is well separated from that7 of the reagent(420nm)at pH9.5.Apparent molar absorptivity of the complex is 2.6×105 lmol-1 cm-1.Beer's law is obeyed in the rang of 0-6μg/10ml for lead(Ⅱ).Tolerance limits were shown for 24 ions.The method established could be applied to the ditect determination of lead(Ⅱ)in sodium chloride with satisfactory result.
    Studies on Michael-Type Reaction of (μ-Mercapto) (μ-Alkylthio) Bis (Tricarbonyliron) (Ⅱ)—Synthesis of (μ-β-Cyanoethylthio) (μ-Alkylthio)-bisTricarbonyliron) and Mechanism of the Michael-type Reaction
    Song Licheng, Hu Qingmei, Zhao Yutian, Wang Jitao
    1986, 7(10):  889-894. 
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    A Michael-type reaction of a series of-(μ-mercapto)(μ-alkylthio)bis(tricar-bonyliron)s,(μ-HS)(μ-RS)Fe2(CO)6,with acrylonitrile can occur under piperi-dine,trifluoroacetic acid or neutral conditions to afford unsymmetrically novel Fe-Scluster complexes,(μ-NCCH2CH2S)(μ-RS)Fe2(CO)6.By elemental analysis,]Rand 1HNMRspectroscopy structures of all the complexes were confirmed and the numbers and ratios of the conformers of some complexes were also determined.In addition,mechanisms of the Michaeltype reaction,being base-induced,self-induced and CF3CO2H-repressed,have been preliminarily discussed.
    Study on Organo Iodosocompounds(Ⅱ)—The Study of the Structures and Properties of Some lodosoaromatic Acids and Esters
    Zhu Shenjie, Zhang Chunhao, Tan Haian, Wang Pingbao
    1986, 7(10):  895-901. 
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    Ortho-Iodosocinnamic acid,ortho-iodosophenylacetic acid,and some ortho-lodosobenzoic esters(methyl,ethyl,isopropyl and tcrt-butyl estcrs)werc synthesized.By comparing their IRand NMRspectra with corresponding iodo compounds and iododichlorides,the intramolecular cyclic structure of these compounds was suggested.According to the IRspectra of ortho-,meta-and para-iodosobenzoic acids and esters,and by comparing their relative activities of oxygenalion of cyclohexane catalyzed by TPPFe(Ⅲ)Cl or TPPMn(Ⅲ)C1the intramolecular cyclic structures of ortho-iodosobenzoic acid and ester were suggested,too.This cyclic structure should form partially in meta-iodosobenzoic acid.
    HPTLC of Tetrahydro-2,4-oisubstituted-1,5-Benzodiazapines
    Lin Zuming, Lu Yingchao, Ma Zhenkun
    1986, 7(10):  902-904. 
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    The trans and cis isomers of some benzodiazapines were separated and quantitated by means of HPTLCtechnique.The conformation of the trans and cis isomers were determined by NMR.
    Analysis of Essential Oil of Siphonostegia Chinensis Benth
    Xue Dunyuan, Li Zhaolin, Chen Yaozu
    1986, 7(10):  905-908. 
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    The chemical compounds of essential oil of Chinese medicinal herb,Siphono-stegia Chinensis Benth,have been analyzed by capillary GC/MS.Thirty five compounds have been identified and estimated They are(%):α-limonene(0.65),1,8-cineole(0.49),3-methyl bicyclo [2,2,2]-octanone(0.81),1 ,cis-2,trans-4-trimethyl-cyclopentane(0.54),l-hexanol(0.70),3-octanol(0.89),n-decanal(0.81),1-octen-3-ol(3.56),menthone(16.50),iso-menthone(0.76),benzaldehyde(0.40),linalool(7.48),pentyl-cyclopropanc(0.54),6-melhyl-(E)-3,5-heptadien-2-one(0.49),trans-caryophyllene(0.89),l-menthol(7.12),pulegone(3.13)α-terpineol(1.50),hexanoic acid(5.12),gcraniol(3.06),benzyl alcohol(3.02),phenethyl alcohol(1.61),1-phenoxy-2,3-propanediol(1.99),AR-methoxybenzaldehyde(0.49),γ-nonalactone(0.40),ccdrol(0.81),6,10-dimethyl-2-undecanone(7.4),eugcnol(0.81),guaiol(6.72),cudesmol(6.77),4-(t-butyl)benzenediol-1,2(2.42),dihydroactinidiolide(0.98),nootkatone(0.58),2,3-dihydro-bcnzofuran(2.54),ascaridolc(0.55),All of these compounds have not been found in the herb previously.
    The Synthesis of O,O-(2,2'-Biphenyldithiophosphates and Tetra-(O,O-Dialkyldithiophosphoryl )-p Benzoquinones
    Hu Bingfang, Hu Zunghua
    1986, 7(10):  909-911. 
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    Eight O,O-(2,2'-biphenyl)dithiophosphates were prepared successfully by the following reaction:Six tetra(O,O-dialkyi dithiophosphoryl)p-benzoquinone were prepared by the following reaction.The steric hindrance of t-butyl derivatives was considered to be responsible for the unsuccessfukness in proceeding the reaction.
    Pulse Catalytic Reaction Kinetics of Toluens on HCeY Zeolite
    Wang Qiuying, Meng Yimin, Han Qingping, Miao Guobin, Liu Nanhui
    1986, 7(10):  912-916. 
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    An HCeYzeolite with SiO2/Al2O3=4.9,exchange degree=78%,and specific surface area=850m2/g was prepared and was used as a catalyst for the demethylation and the disproportionation of toluene.The data of pulse catalytic reaction of toluene on the HCeYzeolite were measured in various temperatures and earring gas flow rates.Experimental results showed that,in the conditions of temperature range of 521-568℃,earring gas flow rate region of 30-60 ml/min,and pressure range of 2.1-3.1 kg/cm2 the main conversion process of toluene on the HCeY Zeolite was demethylation reaction appeared as a first order kinetic characteritic.The apparent activation energy,the adsorption heat and the activation energy of surface reaction were 71.5kJ/mol,34.9kJ/mol and 106.4kJ/mol,respectively.
    The Electrochemical Polymerization of Thiophene in Acid Aqueous Solution
    Chen Yanzhen, Huang Haitao, Tian Zhaowu
    1986, 7(10):  917-922. 
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    People are more and more interested in polythiophene because of its high stability.At present,organic solvent system is still commonly used in electrochemical polymerization of thiophene and its electrochemical study.However,it is more practical to use aqueous solutions instead of organic solvents.The electrochemical polymerization of thiophene in aqueous acid solution is discussed in this paper.In high concentration acid solution,thiophene first undergoes low polymerization,and then the low polymer can be oxidized at the comparatively negative potential to form film.
    A New Goated Wire Ca2+-Ion Sensitive Field-Effect Transistor
    Fu Tingzhi, Huang Depei, Zhu Chunsheng, Ou Huichun, Lu Yuyi, Hu Jin, Zhou Jiarong, Jin Jie, Wang Jinhua, Zhang Guoying
    1986, 7(10):  923-925. 
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    The authors of this paper have developed a Ca2+-ISFETby dissolving just the right amount of calcium bis-(bis-octylbenzene phosphate)with PVCin a tetrahy-drofuran solution,which was coated on platihun-wire(1.8cm long and φ0.4m/m)after adding to it a plasticizer.
    The Line of Limit Cycle in an Open System
    Zhao Lianqing, Chen Zhirong
    1986, 7(10):  926-928. 
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    In the nonequillibrium statistical mechanics of Prigogine or Haken,they recognize that the concentrations changed in periodic reaction belong to a limit cycle in phase plane,that is,in the open system,the system has a phenomenon of self-organization.In this paper,used x y recorder,we first observed the forms of limit cycle from experiment and discussed it.
    The Effect of Patossium and Sodium on the Oxidation and Reduction of Fe3O4
    Li Zhengwen, Ma Ruzhang, Guo Chuntai, Zhou Quding
    1986, 7(10):  929-930. 
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    The effect of patossium and sodium on the oxidation and reduction of Fe3O4 is studied by means of Mossbauer spectroscopy.It is shown that the main effect of patossium and sodium seems to form patossium-bearing or sodium-bearing new compounds in the oxidation of Fe3O4 and the patossium and sodium ions get into the lattices of Fe3O4 and Fe3Oand act as promoting reduction in the reduction.
    A Study of Surface Acid on Mimic Silica Alumina Catalyst(Ⅱ)—Lewis Acid and the Conversion Between Lewis Acid and Bronsted Acid
    Feng Jikang, Li Zhiru Li Song, Li Rongsheng
    1986, 7(10):  931-936. 
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    In this article,by applying EHMOmethod a scries of mimic calculations have been performed for the surface acid of silica and silica-alumina catalyst formed by adding aluminium oxide in silica gel.We have studied the change of Lewis acid strength of mimic catalysts in which silicon have been substituted by aluminium in different position and number.The micromechanism of conversion between Lewis and Bronsted acid also has been studied.The calculations show thai the amount of aluminium in catalyst have a very little influence upon the strength of Lewis acid,even if Al-O-Al structure is formed the Lewis acid strcngth decreased only a little.Then we show theoretically the mechanism of conversion between Lewis acid and Bronsted acid and the nature of Bronsted acidity.Aseries of results from theoretical calculations are in accordace with the experimental results of measurements of Lewis acid and photoelectron spectroscopy.
    Separation of π-System in SCF-MO Methods
    Chen Zhixing
    1986, 7(10):  937-940. 
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    The principles of the separation ofπ-system in SCFMOmethods arc described.The π-resonance integral contribution to energy is proposed as a measure of π-bonding.It is indicated by the π-rcsonance integral contributions and other data of π-system that the C-Cbond in ethane is not a pure single bond but has a small amount of π-bonding The data showing the resemblance of ethane and propylene to butadiene are presented.The details of the algorithm for separating π-system arc presented.
    Study of Steroid Transformation Catalyzed by Polymer-Supported Liquid Membrane Encapsulated Cells
    He Binglin, Li Naihong, Jang Ping
    1986, 7(10):  941-946. 
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    This paper describes the preparation and properties of polymer-supported liquid membrane-immobilized cells of Arthrobactcr simplex which catalyze the transformation of cortisol into prednisolone.The transforming activities of cells immobilized by this method was compared with that of cells immobilized by traditional entrapment method.The results showed that the former were obviously higher than those of the latter,and there was nosapprent difference of mechanical strength between the former and the latter on our operational conditions.The various factors affecting the transformation were studied as well.
    Studies on Ultrasonic Block Copolymerization of Poly(Ethylene Oxide) with Sodium Methacrylic Acid
    Xu Jian, Shen Ye, Xu Xi
    1986, 7(10):  947-952. 
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    The block copolymerization and structure of the copolymer of polyethylene oxide)(PEO)with sodium methacrylic acid(NaMAA)were studied respectively.The ultrasonic copolymerization in PEO-PNaMAAaqueous solution follows the kinetic relationship,-d[M]/dt=k[R]1/6[M].With increasing irradiation time or monomer concentration,the yield and NaMAAcontent in the block copolymer are increased.The chemical and morphological structure of the copolymer were identified by IR,MS,NMR,TEM,DSCetc.,and the results showed that the copolymer obtained was a block one.The yield of the copolymer,formed by irradiating1% PEO-10% NaMAAaqueous solution for a period of 15 min.at 21.5 kHz with 0.7Acathode current,was 24.0%.
    Studies on the Mechanism of the Photopolymerizatibn of Acrylonitrile Initiated by Aniline
    Li Tong, Cao Weixiao, Feng Xinde
    1986, 7(10):  953-958. 
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    We have verified the formation of exciplex in the photopolymerization of acrylonitrile initiated with aniline.There are two routes involed,i.e.either through the excitation of the charge transfer complex of aniline and acrylonitrile or from the excited singlet state aniline and the ground state acrylonitrile to form excited complex which generates two kinds of radicals by proton transfer process,which both will be responsible for the initiation.
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