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    24 December 1986, Volume 7 Issue 12
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    Articles
    Studies on Thermodynamics of Crown Coordination Compounds (Ⅷ)-Calorimitric Titration for Coordination Reaction of 2,3-Benzo-6-Methyl-15-Crown-5 with Alkali Metal Ions
    Shen Mengchang, Luo Qinhui, Feng Xudong, Tu Qingyun, Lu Guoyuau, Dai Anbang
    1986, 7(12):  1055-1060. 
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    The coordination reaction of 2,3-bcnzo-6-methyl-15-crown-5(BCl-15C5)with alkali metal ions was studied in anhydrous methanol by using homemade titr-ation calorimeter of follow-up adiabatic type.The calculated results show that,except the 1:1 coordination compounds,potassium forms 1:2 coordination compounds,but sodium and rubidium do not,and cesium does not react with the crown at all because of its big radius.When methyl was added to crown ring of benzo-15-crown-5,both the stability and coordination reaction enthalpy of 1:1 coordination compounds decreased.This implies that the effect of space hindrance of methyl is stronger than that of increasing electron density on oxygen atom of crown ring.This resembles the effect of methyl to be added to crown ring of benzo-18-crown-6 on coordination reaction studied by us previously.
    Studies on Thermal Stability of Coordination Compounds by Gas Chromatography(XV)-A Kinetic Method for Thermal Decomposition of Surface Complexes
    Wang Xin, Niu Junning, Zhang Haiyan, Xin Xinquan, Dai Anbang
    1986, 7(12):  1061-1066. 
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    This paper deals with the kinetic problem of the thermal decomposition of surface coordination compounds.Considering the different influence of various crystal planes,several surface Maderung constants of MgOwere computed,and the decomposition kinetics of H2C2O4-MgOsystem was treated,as an accumulation of homogeneous surfaces For more complicated systems,according to the energetic heterogeneity on the surface,a kinetic equation has been proposed.where a denotes the degree of conversion,t the time,Athe frequency factor,Ethe initial activation energy,Rthe gas constant,Tthe temperature,n the reaction order,and C1 and C2 arc constants.The calculated results arc in agreement with those of experiments.
    The Investigation of Preparation for Light Rare Earth Nitrates and Their Hydrates
    Tan Qinde Guo Wei, He Ming'an, Gao Shengli, Liu Yilun
    1986, 7(12):  1067-1071. 
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    The various methods for preparing light rare earth nitrates and their hydrates and the drying conditions of these hydrate crystals have been investigataed.The practical methods for preparing Ln(NO3)3nH2O(Ln=La,Pr,Nd,Sm;n=6,5,4,2,1)and La(NO3)3 have been presented.
    Degradation Method for Preparing Organo-Arsenic and-Antimony Polytungstates, and Comparative Study of Corresponding Polymolybdates
    Gu Yidong, Liu Benyao
    1986, 7(12):  1072-1074. 
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    B2[(Me2As)Mo4O15H]and B4[(RP)2Mo5O21]types of compounds were first prepared by M.T.Pope in1975 and 1976[1].Thereafter,the preparation of polytungstates and polymolybdates with organo-phosphonates and-arsonates "handles" has been in rapid progress[2].The potential uses of such compounds as antiviral and biological agents have been noted.
    The Separation and Identification for Non-Ionic Surfactant of Type of Fatty amide Poloxyethylene by HPLC-NMR IR Method
    Shi Jingjiang, Liu Yufen, Zheng Yongjie, Wang Zhen, Wu Xiaohui, Sang Changchun
    1986, 7(12):  1075-1080. 
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    The total components of non-ionic surfactant of type of long chain fattyamide-polyoxyethylene both with wide molecular weight distribution range and larger dispersion degree have been well separated by HPLCmethod under optimum separating conditions.In the case without the standard ,the fairly satisfactory reseach results of this kind of sample have been obtained by preparation of the main fractions and the aid of NMRand IRidentification.Multi-propramming eiution and change of flow rate are suitable to the analysis of complicated components.This method has the characteristics of fast speed,high efficiency,simplicity and trustworthy.
    Polymer Surfactants as Analytical Reagents-Synthesis and Analytical Properties of PPOTA and PPOCA
    Liu Kunyuan, Xie Hui, Pan Gulan, Yu Ruqin
    1986, 7(12):  1081-1084. 
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    Two new polymer surfactants polypropylene oxide-a-tetradecyldimethylammo-nium chloride(PPOTA)and polypropylene oxide-a-cetyldimethylammonium chloride(PPOCA)have been synthesized,which possess the characteristics of both cationic and nonionic surfactants.The properties of PPOTAand PPOCAwere investigated.The synthesized surfactants can be used as sensitizing and solubilizing reagents for spectrophotometric analysis.Some examples of micellar improved spectrophotome-tric systems such as Sc(Ⅲ)-CAS,Ge(Ⅳ)-PFand Ni(I)-CASwere given.
    Studyies on the Adsorptive-Complex Wave of Cadmium(Ⅱ)with Thiosemicarbazide
    Hu Naifei, Li Qilong, Lin Shuchang
    1986, 7(12):  1085-1089. 
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    In the supporting electrolyte containing4.0×10-3Mthiosemicarbazide(TSC)and 0.04Mpotassium hydrogen phthalate(pH=4),a sensitive derivative peak wave has been obtained by using single-sweep oscillopolarography.The peak potential is-0.65V(SCE).The change of peak height with the concentration of cadmium(Ⅱ)is linear in the range from 8.9×10-8 to 3.6×10-6M.The mechanism of the wave has also been studied in detail.The chronocoulometric study shows that in the presence of TSCthe adsorption of Cd(Ⅱ)on the surface of Hg electrode is direct adsorption of Cd(Ⅱ)-TSCcomplex and the adsorbed species is Cd(TSC)2+.
    The Purification of Organic Solvent in Li Cell and Its Effect
    Ding Yunchang, Wang Zhongfeng
    1986, 7(12):  1090-1093. 
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    Studies on Li cell have made great progress these years,which brings study and use of organic electrolyte solutions.In the development and use of the cell,people show great interest in the purification of the solvents which make the electrolytic solutions,and its effect.Because of the chemical specific property of Li,people pay close attention to removing water from the solvents.The propylene carbonate(PC),1,2-dimethoxyethene(DME),tetradrofuran(THF)and 4-butyrolactone(BL)are usually used as solvent to prepare electrolyte solution for Li cell.This paper is about the study on purification of organic solvent and its effect.Experiments show that the means of purification in the paper may produce good effect of removing water.
    Solid-State Photochemistry of 2,5-Cyclohexadienones(Ⅱ)
    Meng Jiben, Matsuura. T, Ito. Y
    1986, 7(12):  1094-1097. 
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    Photochemical reaction of 2,4,6-tri-t-butyl-4-methoxy-2,5-cyclohexadienone in the solid-state has been investigated.Photoketone,photophenol,lumiketone were obtained.The ratios of products varied with temperature.In solution,the ratio was not effected by temperature.Irradiation of crystals of 2,4,6-tri-t-butyl-4-methoxy-2,5-cyclohexadienone with filter of solution of NaNO2,the lumiketone was obtained almost quantitative yield.If the mixture of lumiketone containing a small amount of naphthalene is irradiated,the ratios of products varied with amount of naphthalene.
    Studies on Michael-Type Reaction of (μ-Mercapto)-μ-Alkylthio) Bis (Tricarbonyliron)(Ⅲ)-Synthesis of (μ-3-Oxobutylthio)(μ-Alkylthio) Bis (Tricarbonyliron) and Reactivity of α,β-Unsaturated Substrates
    Song Licheng, Zhao Zhengyun, Hu Qingmei, Wang Jitao
    1986, 7(12):  1098-1103. 
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    Amichael-type rea ction of a series of(μ-mercapto)(μ-alkylthio)bis(tricarbony-liron)s,(μ-HS)(μ-RS)Fe2(CO)6(A),with methyl vinyl ketone can take place to give unsymmetrically novel Fe-Scluster complexes containing 3-oxobutyl group,(这里有图片19861210-1098-1.gif).This Michael reaction is characterizedby.
    Synthesis of Benzoxepinoquinolinone
    Liu Shouxin, Gao Yongjun, Jiang Guiji
    1986, 7(12):  1104-1108. 
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    1-beazoxepino[3,4-b] quinolin-13(6H)-one(14)and its halogen and alkly-derivatives(15-18)were synthesized through cyclization of 2-[(un)substituted phenoxy]-3-quinilinccarboxylic acids(9-13)in the presence of P2O5-H3PO4 or PPA.The acids(9-13)were obtained from the corresponding ethyl esters(4-8)which were prepared through refluxing ethyl 2-bromomethyl-3-quinolinecarboxylate(2)with phenol or substituted phenol in sodium ethoxide ethanolic solution.Compound(18)reacted with CuCNto give compound(19)which was hydrolyzed to give carboxylic derivative(20).The structure of 19 new compounds have been confirmed by element analysis,IRand NMR.
    The Synthesis,Reaction and Catalytic Activity of Morpho-line Coordinated Molybdenum and Tungsten Carbonyls
    Zhang Zhengzhi, Wang Xukun, Zhao Weijun, Zhang Shuji, Fang Yanquaa, Liu Maoping
    1986, 7(12):  1109-1111. 
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    Aprocedure for large amount of preparation of cis-bis(Lewis base)coordinated molybdenum and tungsten carbonyls is proposed.The structures of these new compounds are discussed and their exchange reaction with tertiary phosphines as well as their catalytic activity for carbonylation of methanol was studied.
    The Static Dielectric Constant of Salted Solutions
    Zhu Jianjun, Lu Jinsuo
    1986, 7(12):  1112-1117. 
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    Applying the definition of extra polarization and Mori's Brown motion equation,we got the secular motion equation for extra polarization from the nonequi-librium standpoint.We have solved the secular Eq.with the help of the assumption of equal effective ionic electric field.It shows not only the ion's radius but also the solution structure and solvent properties are responsible for the per-mittivity decrement.Using the present result,calculations are carried out for the systems of LiCl-CH3OH,NaCl-CH3OH,NaI-CH3OH,NaCl-H2O,LiCl-H2O ,KCl-H2O,NaI-HCONH2,Comparison among the continuum theory,molecular theory and ours is made,it shows our result is better to the salted system of alchol and water
    The Determination of Heterogenous Rate Constants in the CV Oxidation of Adenine
    Zhou Duanci, Xie Yiheng
    1986, 7(12):  1118-1121. 
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    The desorption of adenine on glassy carbon electrode(GCE)was observed in the presence of sulfate and the adenine oxidation on GCEwas exclusively controlled by diffusion.The heterogeneous rate constant for electrochemical oxidation of adenine,KEp ,and its potential dependence were also determined by usingGVdata and chronoamperometric diffusion constant.
    The Quantum Calculation for the Structural Rule of the Transition Metallic Heteroboranes
    Li Zhiru, Li Qianshu, Tang Aoqing
    1986, 7(12):  1122-1126. 
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    In this paper we have calculated various polyhedral skeletons of the transition metallic heteroboranes,FenB6-n(n=0,1,...,6)by using the Hoffmann's program of EHMOmethod,verified and discussed the structural rule of the thansition metllic heteroboranes proposed by us.BMO+NBMO=4n1+9n2-Fwhere BMO+NBMOstands for the number of valence bonding and non-bonding molecular orbitals,n1 and n2 are respectively the numbers of main group and transition metal atoms in the skeleton of a heteroboranes,and Fis the number only depending on the geometry of the skeleton,and discussed some properties of the skeletons.As example,we also calculated C6H5FeB9C2H11 and its skeleton by the same method to compare each other.
    A Study on the Mechanism of Intramolecular Electron Transfer and Dehalogenation of Halogenated Benzonitrile Anion Radicals
    Ye Song, Dai Shushan
    1986, 7(12):  1127-1131. 
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    The mechanism of intramolecular electron tranffer and dehalogenation of halogenated benzonitrile anion radicals was studied by INDOmethod.Calculations show that intramolecular electron transfer and dehalogenation are synchronous processes.The rates of dehalogenation arc found to be dependent on the ease of electron transfer and the energy level of antibonding MOof C-X bond.
    The Adsorption Behaviors of Typical Surface-Active Substances on Hg, Cd(Hg) and Pb(Hg) Electrodes
    Qu Jin, Liu Tianqing
    1986, 7(12):  1132-1136. 
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    The interfacial capacity-potential curves of Hg,Cd(Hg)and Pb(Hg)electrodes and the desorption potentials" on the three electrodes in12 typical surface-active organic substances in1M KC1 were measured by DD-1 typle electroplate parameter measurement meter.As anodic soluble potentials of Cd(Hg)and Pb(Hg)electrodes are more negative,the desorptions F-,Cl-,Br-were not found.It was found that the sequence of surface activities of I-and the surface activities of same surface-active substances on the three electrodes usually follow Hg>Pb(Hg)>Cd(Hg).Given results show.The difference of desorption potentials on the three electrodes in same concentration and same surface-active substances was less 10mV.It was showed that the surface characters of Cd(Hg)and Pb(Hg)at the desorption potentials were as same as that of Hg.
    Study on PVC Membrane Electrode (Ⅲ)-Development of a Tetrachloroantimony (Ⅲ) Complex Anion-Selective Electrode
    Guo Dingli, Xie Zhiwei, Gao Huashou
    1986, 7(12):  1137-1139. 
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    Anew chloroantimony complex anion-selective electrode of PVCmembrane based on the associated substance of quaternary ammonium salt and tetrachloro-antimony(Ⅲ)complex anion is discribcd.
    Investigation on Solid-State Polycondensation Nylon-1010 Salt
    Zeng Hanmin, Chen Haining
    1986, 7(12):  1140-1145. 
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    In this work the kinetics of the solid state polycondensation of nylon-1010 salt and its crystalline morphologies have been studied by the use of a number of techniques including determination of conversion rate and molecular weight,IR,elemental analysis,X-ray diffraction,polarized light microscopy,DSC,and SEM.The experimental results indicated that nylon-1010 salt is a kind of zwitter-ion crystalline,the conversion rate and molecular weight of nascent nylon-1010 are dependent on the reaction temperature and the innert gas N2 flow.It was found that reaction temperature remarkably influence the course of the solid-state poly-condensation.The morphologies of like-fibril structure of formed nascent nylon-1010 have been discussed.It should be pointed out that the reaction temperature is slightly below the melting point of nylon-1010 salt which makes it possible for solid-state polycondensation to appears to have like-melt state reaction features.
    Study of Solid State Polymerization of Bis (p-Toluene Sulfonate)of 2,4-Hexadiyne-1,6-Diol with Laser Micrometry
    He Pingsheng, Li Zhichao, Chu Feng, Peng Jianbang
    1986, 7(12):  1146-1149. 
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    Bis-(p-toluene solfonale)of 2,4-hexadiyne-1,6-diol(TS)monomer is a macroscopic single crystal which can polymerize into polymer single crystal(PTS)without changing its crystal mode under heating.The macroscopic dimensions of TScrystal during solid state polymerization have been monitored by means of laser micrometry.The change of parameters of unit cell during polymerizing TSinto PTScan be estimated from the measuring of the dimensions of the single crystal.The results show that c axis of unit cell which is the direction of forming PTSmacromolecular chain contracts during whole polymerization,but both a and b expand firstly,then contract.
    Syntheses of New Tetraphenylphenylorganosilicon Compounds
    Chen Jianhua, Feng Shengyu, Du Zuodong
    1986, 7(12):  1150-1155. 
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    The following new tetraphetlylphenylsilicon compounds have been synthesized by Diels-Alder reaction;(Ⅰ)bis(tetraphenylphenyl)tetramethyldisiloxane,(Ⅱ)tetraphenylphenylvinyltetramethyldisiloxane,(Ⅲ)tetraphenylphenylmethyldichloro-silane,(Ⅳ)tetraphenylphenylheptamethylcyclotetrasiloxane,(Ⅴ)tetraphenyl phenyl-methylsilanediol,(Ⅵ)trimethyltri(tetraphenylphenyl)cyclotrisiloxane,(Ⅶ)etramethyltctra(tetraphenylphenyl)cyclotetrasiloxane.Structure and composition of compounds(Ⅰ-Ⅶ)were determined by spectral analyses.
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