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    24 September 1987, Volume 8 Issue 9
    Articles
    Studies on the Interfacial Properties of Liquid-Liquid Extract ion(Ⅲ)--Interfacial Properties of Primary Amine N1923in the Extraction Systems
    Gai Haifa, Gao Zili, Sam Sixiu, Shea Jiaglan
    1987, 8(9):  767-772. 
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    The iaterfacial adsorption characteristics of primary amine N1923in liquid-liquid extraction systems have been studied. It may be concluded from the experimental results that N1923is adsorbed at the interface in the form of single-molecule. The adsorbability depends on the temperature and the nature of diluents. The experimental results showed that the weaker the polarity of diluent, the stronger the adsorability, and the higher the temperature, the weaker the adsorability. The influence of the aqueous medium concentration on the interfacial adsorption characteristics is not very obrioas. The relation between the adsorption properties of N1923and its extractability also discusied.
    Study on the U(Ⅳ)-U(Ⅵ) Redox Displacement Chromatography (Ⅵ)--Cationic Ion Exchange Bed-Ti(Ⅲ)-FeCl3-Carboxylic Acid System
    Qiu Ling, Chen Jingren, Zhang Minquan, Zhang Wenbo
    1987, 8(9):  773-778. 
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    Cationic ion exchange U(Ⅳ)-U(Ⅵ) redox displacement chromatography with citric, tartaric lactic, succinic,iminodiacetic acid and acetylacetone as complex agent was studied. The possibility and way to obtain high enrichment factor of uranium isotope separation as carboxylic acid is used as complex agent was mainly dealted. From the results it may be expected to increase the enrichment factor to (8.5-9.0)×10-4, approaching the level offered by ion exchange process, if carboxylic acid is correct selected and its concentration as well as displacement ion concentration are properly controlled.
    Ternary Complexes of Ce(Ⅳ) and Th(Ⅳ)
    Zhu Wenxiang, Yin Shouyi, Zhao Jizhou
    1987, 8(9):  779-783. 
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    Two ternary complexes of Ce(Ⅳ) and Th(Ⅳ) were isolated. Their properties have been studied with conductometry, thermal analysis and absorption spectro-scopy. FT-IR difference spectrum technique was also employed in examination of the complexes.
    A Study on the Oxidation-Reduction Characteristic of the Bimolybdenum Complex Compound
    Sun Wentao, Zhang Zhigui
    1987, 8(9):  784-786. 
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    The cyclic voltammogram of bimolybdenum complex compound is reported. It is shown that there are a pair of redox peaks and one reduction peak in the cyclic voltammogram. The results indicate that the redox peak pair is corresponding to the redox reaction of Mo[S2CN(C2H5)2]4+, which is semireversible, but another reduction peak is corresponding to the reduction reaction of MoCl6-, which is irreversible.
    A Selective Determination of Molybdenum in the Presence of Large Amount Tungsten by the Difference of Solutional State
    He Xiwen, He Huarui, Shi Huiming
    1987, 8(9):  787-792. 
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    A simple selective spectrophotometry has been developed for determination of molybdenum in the presence of tungsten based on the difference of polymeric behavior and complex ability. In the present paper, it is demonstrated how increase difference of solutional state between molybdenum and tungsten. It has been found that the method do not affect the absorbance of complex by forming molybdenum with bromopyrogallol red (BPR) but the complex of tungsten would almost become to fide.The method was applied to determine the micro amount of molybdenum in the tool steel with Satisfactory results.
    Homogeneous Voltammetric Immunoassay of Diphtheria Toxoid and Diphtheria Antitoxin
    Hu Yinhua, Tie Feng, Li Qingman
    1987, 8(9):  793-796. 
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    Diphtheria toxoid is denatured in 0.1M NE4Cl-NH3·H2O basal solution with pH9.4, yielding a cathodic and an anodic polarographic peaks at-1.50 and-1.46 V(vs.SCE) respectively.The cathodic and anodic peak heights vary linearly with diphtheria toxoid concentration over the range of 2.5 to 180 μg/ml by single sweep polarography; and even as low as 0.3μg/ml, diphtheria toxoid could be detected by differential pulse polarography. The decreased peak current value of diphtheria toxoid is proportional to diphtheria antitoxin present due to immuno-chemical binding reaction in the range of 2.5×10-6to 5×10-5IU/ml,which determines diphtheria antitoxin level homogencausly. The assays are sensitive specific, resproducible in operation The anodic peak has been applied to the determination of diphtheria toxoid in the triple vaccine.
    Studies on Adsorptive Complex Wave of Lead -1,10-Phenanthroline
    Zeng Yonghuai
    1987, 8(9):  797-801. 
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    In a supporting electrolyte containing 2×10-5Mphen, 0.06MHAc-0.14M NaAc and at pH5.1, we obtained an adsorptive complex wave of Lead-phen by Single-Sweep Polarography. It was found that the peak potential of the derivalivc wave is -0.49V (vs.SCE) and limit of detection for lead is 2.5×10-8M.We determined the composition of the complex which is 1:1 Pb(Ⅱ)-phen and confirmed that the wave is an adsorptive complex wave. The electrode processes may be presented as follow:Pb2++ phen⇔Pb(phen)2+ Pb(phen)2+⇔Pb(phen)2d2+ Pb(phen)2d2++2e+ Hg⇔Pb(Hg)+phen
    The Bactericidal Activity of Some 2-Amino-5-Alkyl-1,3,4-Thiadiazoles
    Hu Bingfang, Li Zengmin
    1987, 8(9):  802-806. 
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    With the purpose of seeking more effective, less hazardous bactericides against rice leaf blight, there were synthesized sixteen 2-amino-5-alkyl-l,3, 4-thiadia-zoles (Ⅰ) (among them seven new compounds) and eleven O,O-diphenyl phosp-horyl amides of various 2-amino-5-alkyl-1,3,4-thiadiazoles (Ⅱ), as well as four O,O-dialkyl-S-(N-l,3,4-thiadiazole) aminomethyldithio-phosphorates (Ⅲ). All these compounds were tested against xanthomonas campestris pv.oryzae or Agrobacterium tumcufacenec in vitro. The biological evaluation results showed that compounds of types Ⅰ and Ⅱ were active and the activity was correlative with the length of the n-alkyl at 5 position.
    The Study of Heterocyclic Organophosphorus Comdpunds(Ⅵ)--Synthesis of 2-Thio(or Zero)-2-Carbalkoxy-1,3,2-Benzodioxaphospholes
    Li Yugui, Liu Tingyang, Shen Yongfang, Yang Gungwei, Yao Yunsheng, Qiang Zhaolin
    1987, 8(9):  807-812. 
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    Four P(Ⅲ) benzodioxaphospholes (Ⅰ1-4) and seven P(Ⅴ) benzodioxaphos-pholes(Ⅱ1-7) were preparaed. The spectrum characteristics were reported. It was considered that the ratio rate of the E, Zstereoisomers of ethenyl was changed with the P(Ⅲ) valent state and the red shift in IRof the compounds Ⅱ1-3were observed.
    A New Method of Synthesis of α-Bromocinnamamides
    Wang Shuyu, Liu Weiqin, Li Renli
    1987, 8(9):  813-818. 
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    α,β-Dibromophenylpropionyl chloride reacting with organic amine (lower molecular weight) can yield a pair 01 cis and trans geometric isomers of α-bromocinnamamide. But the relative amounts of cis and trans isomers are influenced by the ratio of the amine employed. On the other hand the substituents on the phenyl ring and the solvents used in the reaction have some influence too. By this method and preparative TLC, we isolated and obtained eight pairs of geometric isomers including m-chloro-α-bromo-N-sec-butyl-cinramamides, p-bromo-α-bromo-N-isopropyl-cin-namamides, etc.
    Studies on the Meerwein Arylation Reaction(Ⅰ)--Arylation of N-Vinylphthalimide
    Hu Hongwen, Pan Yi, Xu Jinghua
    1987, 8(9):  819-822. 
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    N-Vinylphthalimide was treated with aromatic diazonium chlorides ArN2+Cl-<Ar=o-BrC6H4-;p-BrC6H4-;o-ClC6H4-;p-ClC6H4-; 2, 4-Cl2C6H3-; 2,6-C12C6H3-;2,4,6-Br3C6H2-; p-CH,COC6H4-; m-NO C6H4-) in the presence of cuprous chloride to give the corresponding N-(2-ary1-1-chloroethyl) phthalimide.The latter compounds were transformed to N-(2-arylvinyl)phth--alimide by refluxing with N, N-diethylaniline.
    The Construction of a Constant Temperature Environment-Continuous Titration Calorimeter and the Improvement of Thermogram Analysis
    Chen Rongti(Y. T. Chen), Gu Zongxin, Chen Xuemin
    1987, 8(9):  823-828. 
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    A constant temperature environment-continuous titration calorimeter has been constructed in our laboratory with the components commercially available on the market. The tenability of this instrument has been tested and its sensitivity determined to be 9.91×10-5kmm-1. This calorimeter was chemically calibrated with the neutralization of strong acid and base (HCIO4+NaOH) and the value of △HN0=-13.341 kcalmol-1was obtained which is quite agreeable with the literature. The results obtained from the measurement of the thermodynamic properties of Ag(Ⅰ)-pyridine complexation reactions conform nicely with those cited in the literiture. The data evaluation procedures have also been improved in the analysis of thermogram.
    The Characteristics of Effect of Intraparticle Diffusion on the Kinetics of Redox Mechanism
    Jin Yon, Yu Qiqaan, Liu Meiziao
    1987, 8(9):  829-834. 
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    The kinetics of oxidation of methanol to formaldehyde over Pb0.88Bi0.06La0.02Mo/SiO2catalyst was described by Redox mechanism of two stages.When the particles of catalyst increased to 3 mm in diameter, the effect of intraparticle diffusion strongly depended on the rate of oxidation of methanol to formaldehyde. The effectiveness factor of catalyst was determined by experiments to be 0.38-0.73.The kinetic equation of Redox mechanism in the presence of intraparticle diffusion of oxygen was interpretated by the theory of intraparticle diffusion and proved by experiments.The apparent activation energies of oxidation of methanol in the presence of intraparticle diffusion of oxygen were determined and interpreted by the kinetic experiments and a theoritical equation.
    Surface Adsorption and Micelle Formation of 9-Ethoxy--Fatty Alcohols with Gaussian Distribution of Carbon Chain Length in Aqueous Solution
    Xia Jiding, Sun Yan, Zhou Heyun
    1987, 8(9):  835-838. 
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    The effects of different carbon chain length with Gaussian distribution of 9-ethyoxy-fatty alcohol(AE9) on the surface adsorption, micelle formation were studied. Experimental results indicate that regular solution theory with nonideal miximg rule seems to be more reasonable than ideal mixing in calculating therm-odynamic parameters of this system. The efficiency and effectiveness of surface tension reduction and synergestic effect of mixed AE9solution can be increased by adjusting properly the carbon chain length distribution of polyoxyethylenated fatty alcohols.
    Photophysical and Photochemical Properties of Diacetonitrile-Bis-(2,2'Bipyridine) Complex of Ruthenium(Ⅱ)
    Chen Zhong
    1987, 8(9):  839-841. 
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    The pholophysical and photochemical properties of the complex Ru(bpy)2-(CH3CN)2(PF6)2in solvents and acidic solution were investigated. The complex exhibits stronger luminescence at 77K in solvents, The emission maximum is at 54Cnm and a second weaker band is at 580nm in methanol-ethanol. They are characterized by a band near G50nm and a second weaker band at 590nm in 1N H2SO4rnethanol.Emission lifetime is about 210 ns in methanol solution at 10℃. The complex to be irradiated at 254nm,283nm and 414nm in 0.lNH2SO4solution results in pseudo-first order photosubstitution reaction, producing cis-Ru(bpy)2-(CH2CN)(OH2)2+, the last photoprcduct is cis-Ru(bpy)2(CH2)22+. The quantum yields of disappearance for the complex are reported at irradiation wavelengths.
    The Linear Themodynamical Relationships in Coordination Compounds--Linear Free Energy Relationships, Linear Enthalpy Relationships and Linear Entropy Relationships in the Ternary Mixed Coordination Compounds Formed from Amino-acids and 1,10-Phenan
    Chen Ziyuan, Wang Shaohua
    1987, 8(9):  842-844. 
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    The stability constants of ternary mixed ligand coordination compounds formed from some amino-acids (serine, valine, alanine and α-amino-isobutyric) and 1,10-phenanthroline with Cu(Ⅱ) were determined by pH-meterically at 25±0.1℃, 35±0.1℃ and 45±0.1℃ in the presence of 0.16M KNO3Linear relationships not only exist between the stability of ternary mixed ligand coordination compound and the base strength of ligands but also exist between the formation enthalpy of coordination compounds and the protonalion enthalpy of the ligands and between the formation entropy of coordination compounds and the protonation entropy of the ligands as well.
    Studies on the Radiation Chemistry of the Aqueous Solution of 1,8-Dihydroxy-Anthraquinone-β-D-Glucoside
    Sun Hai, Yuan Rongyao, Wu Jilan
    1987, 8(9):  845-850. 
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    In this paper the radiolysis of the aqueous solution of 1, 8-dihydroxy anthra-quinone glucoside has been investigated, the results are as follows.1.OH radical reacted with 1,8-dihydroxy anthraquinone-β-D-glucocide leading to the radiolysis of glucoside but no glucosidic bond rupture was found.2.Two radiolysis products have been obtained. Product may be an aliphatic alcohol which comes from the decomposition of glucose radical. ProductⅡ is still a glucoside which may be a trihydroxy anthraquinone glucoside.3.Using competition kinetics we have got kOH·+glucosidc=2.9×109mol-1s-1.
    Kinetics of Methyl Methacrylate Bulk Radical Polymerization (Ⅰ)--Conformation and Concentration of Radical and Propagating Constant kp
    Tian Yuan, Zeng Yingguang, Wang Guobing, Qiu Zuwen, Shen Jiacong
    1987, 8(9):  851-855. 
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    By using TM110cavity and 2mm sample tube, the ESRspectra of the propagating radical in the polymerization system of methyl methacrylatc were recorded. The concentration and conformation of radicals and the propagating constant kpwere measured.The results showed that the propagating reaction was a diffusion controlled process.
    Polymerization of Polypropylene Oxide in the Presence of a Triethylaluminium-Monoalkyl-Phosphate Catalytic System and Study of 13C-NMR Spectra of Polymer
    Ye Hongwei, Wang Xinling, Hu Gengyuan, Yang Shilin
    1987, 8(9):  856-858. 
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    A catalytic system, (C2H5)3A1/ROPO(OH)2, exhibits higher activity in the polymerization of propylene oxide(PO), The polypropylene oxide and its crystalline acetone-insoluble fraction were determined by the 13C-NMR.In the 13C-NMR spectra of the PPO, we discovered the most direct way of identifying the two kinds of lines. As an illustration, the two kinds of lines in 13C-NMR were due to results of methine and methylene carbons of a high molecular weight PPO, respectively. Chemical-shift and split of four configuration of isotactic, heterotactic and syndiotactic have already been compared for the PPOwith different catalytic systems, (C2H5)3A1/ROPO(OH)2, (C2H5)3A1/H3PO4,and(C2H5)3Al/AcAc/H2O.
    Research of a Silicone Emulsion
    Liu Hongyun, Wang Xiangxiao, Du Zuodong, Wang Xiujie, Zhou Yuqi, Shi Weizhen, Ma Juli
    1987, 8(9):  859-861. 
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    Reactive periods were determined for emulsifying polymerization of D4; put forward a emulsifying polymerization method about to add a initiating emulsion and the effect for every factors on the emulsifying polymerization and stabilization of the emulsion was discussed.