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Table of Content

    24 January 1985, Volume 6 Issue 1
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    Articles
    Calorimetric Study on LaNi4M(Ni, Cu,Fe)-H2 Systems
    Shen Panwen, Wang Genshi, Song Deying, Lu Shuqin
    1985, 6(1):  1-6. 
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    The relative partial molar enthalpies △HHα→β for absoption of H2 By LaNi5, LaNi4Cu and LaNi4Fe have been measured respectively, using a calorimeiric system[1] at 298.3K. The values obtained are -3.590± 0.036, -3.905±0.038 and -4.049 ±0.041 Kcal/molH. Their △GHα→β have been also measured and their △SHα→β have been calculated. △HHα→β of LaNi5 is in agreement with that cited in the literature[2] while those of LaNi4Cu and LaNi4Fe measured by calorimetry have not been reported as yet in literature. The lattice parameters of LaNi5, LaNi4Cu and LaNi4Fe have been determined by X-ray diffraction analysis. The relations between △HHα→βHα→β, △GHα→βHα→β and unit cell volume Vare:△HHα→β= -0.2509V +18.25△GHα→β= -0.2258V + 20.02.
    Hydrolytic Polymerization of Chromium(Ⅲ) Ion(Ⅴ)——The First and Second Hydrolysis Constants of Cr3+
    Luo Qinghui, Shen Mengchang, Ding Yi, Dai Anbang
    1985, 6(1):  7-12. 
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    The chromium(Ⅲ) ion is of characteristic by hydrolysis reaction. Its second hydrolysis-product Cr(OH)2+ always coexists together with polynucl-ear species, but this complicated case was not takeninto account while determinating hydrolysis constant of Cr(OH)2+. Therefore the result obtained by previous authors is unsatisfactory. We proved first by calorimetric titration that the first hydrolysis product CrOH2+ can exist alone, but Cr(OH)2+ can not within certain range of pHvalue and furthermore obtained the first and second hydrolysis constants by curve-fitting under considering the coexistence of mono- and polynuclear species. The result is as follows: lgβ11 = -4.15±0.04, lgβ21 = -8.40 ±0.03. The comparision with the previous results has deen made.
    Synthesis and Characterization of a New Water Soluble Cobalt Porphyrin Coordination Compound
    Cao Xizhang, Xiu Zhengkun, Wang Maolian, Liu Zheirong, Yu Lianxiang
    1985, 6(1):  13-17. 
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    In this paper a new water soluble cobalt porphyrin coordination compound, Co·C56H60N8I4·6H2O (CoTAPPI), was prepared and characterized by UVabsorption spectra, TGand DTA, IRspectromelry, Raman spectro-metry, ESRspectrometry. Which revealed that this compound has an ability of carrying oxygen.
    Factor Examination on the Gas Chromatographic Determination of Trace Amount Chromium and the Measurement of Chromium in Human Hair
    Chen Weijie, Qin Fu, Zhang Tieyuan
    1985, 6(1):  18-22. 
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    The principal conditions of GCdetermination method for subnanogr-am Cr through Cr (Ⅲ)-trifluoroacetylacetonate were sdudied in detail. Aplan of balanced design was selectd for seven factors each with two modified conditions, such that the sensitive factors most likely to influence the results were picked out, improved and emphasized in the procedure. The analytical results for tap water were compared with neutron activation analysis. The coefficient of variation for 1 to 10 ppb Cr in water is ≤3% (n≥6), recovery is in the range of 95-100%, and the 3σ limit of detection is 0.014ppb (n = 22). Four batches of hair samples were analyzed, the Cr content is in the range of 0.42-2.18 μg/g and the coefficient of variation (n = 5) being 10-3% accordingly.
    Simultaneous Spectrophotometric Determination of Palladium, Rhodium and Platinum
    Fang Guozhen, Zhang Yugui
    1985, 6(1):  29-32. 
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    Asimple, accurate, sensitive, and reliable . method for simultaneous spectrophotometrie determination of palladium, platinum and rhodium in the their mixtures has been suggested. The method involves first, in the medium of EDTA-NaOHthe determination of palladium as the red PARcomplex without interference from platinum, rhodium and many foreign cations. Then, by the use of the perchloric acid and stannous bromide, both the excess PARand its palladium complex were decolorized.
    A Study of the Ternary System of Titanium(Ⅳ)-Stilbazo-Cetyl-Trimethyl Ammonium Bromide and Its Application in Spectrophotometric Determination of Titanium
    Chen Yushou, Chen Minghe, Cai Yanping
    1985, 6(1):  33-35. 
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    In a weak-acid solution, titanium was found to be able to react with stilbazo and cetyl-trimethyl ammonium bromide(CTMAB), forming a red ternary complex. The wavelength of maximum absorbance for the complex was 520nm.The molar ratios of the components in the complex are estimated to be Ti (Ⅳ): stilbazo :CTMAB = 1:3 : 6. The present method can be applied to the determination of trace Ti in water. A 5cm cell was used in the spectrophotometric determination, the molar absorptivity was 1.1×105 at 520 nm. The calibration curve well follows Beer's law in the range from 0 to 0.75 μg of Ti (Ⅳ) in 25 ml solution under the above condition. It was found that the method proposed in this work had high sensitivity and gave gratifying result in the determination of Ti (Ⅳ) in water.
    Studies on the Chemical Constituents of the Chinese Medicinal Herb Anemone Raddeana Regel(Ⅲ)
    Wu Feng'e, Zhu Ziqing
    1985, 6(1):  36-40. 
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    The Chinese medicinal herb, Anemone raddeana Regel, has been used for treatment of rheinnatism and phlebits etc. in folk medicine. Anew saponin R1, which was named raddeanin B, and glucose as well as cane sugar have been isolated from this plant.By spectroscopic and chemical methods, it has been identified as 3-O-[α-L-rhamnopyranosyl-(1→4)-α-L-arabinosyl]-oleanolic acid. It has not been isolated previously from any plant source.
    The Reaction of Bis(O,O Diethylthiophosphoryl)Disulfides with Mercuric Chloride
    Hu Bingfang, Chen Wanyi
    1985, 6(1):  41-44. 
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    Bis(O,O-diethylthiophosphoryl)disulfide and bis(O, O-dibutylthio-phosphoryl)disulfide reacted with mercuric chloride in 1:1 or 1:2 mole ratio at room temperature to give addition compounds.
    Synthesis of 2'-Hydroxy-1',3'-Xylyl Crown Ethers
    Wang Defen, Jiang Peihua, Hu Hongwen
    1985, 6(1):  45-48. 
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    Condensation of 4-chloro-2, 6-bis(hydroxymethyl)-l-methoxy benzene and 4-pheny 1-2, 6-bis(hydroxymethyl)-l-methoxy benzene with the appropriate oligoethyleneglycol ditcsylate in anhydrous tetrahydrofuran containing potassium t-butoxide produced the methoxy crown ethers 5-7.Ref-luxing 5-7 with anhydrous lithium iodide in dry pyridine gave 2'-hydroxy-1', 3'-xylyl crown ethers in 85-89% yield.
    Study on the Organometallic Compounds of Transition Metals Containing Pentahaloaryl Ligands(Ⅰ)——Synthesis and Reactions of Bis(Diphenyl-Alkylphosphine)Pontachlorophenylnickel Chloride
    Wang Xukun, Zhang Zhengzhi, Wei Dong
    1985, 6(1):  49-53. 
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    The compounds of general formula (Ph2PR)2Ni(C6Cl5)Cl(R = CH3, C2H5, n-Pr, n-Bu) were synthesized. Their chemical reactions with inorganic halides and pseudohalides, as well as organolithium reagent and al-kynyl compounds were investigated. Through these reactions, a series of new organonickel compounds have been prepared and the scope of applications of some reactions has been expanded.
    Research on 2,5-Disubstituted Oxadiazoles
    Pan Jiaxing, Liu Yadong, Gao Zhenheng
    1985, 6(1):  54-58. 
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    2-Phenyl- and twenty five of 2-(substituted phenyl)-5-(4'-biphenyl-yl) oxadiazoles were synthesized. The. m.p., λmax of UVabsorption spectra and fluorescence emission spectra, fluorescence quantum yield as well as laser properties of the compounds are given in tables. It is found that seventeen of the compounds give higher conversion efficiency than PPOin near UVregion.
    Preparation of Diazomethane by Phase Transfer Catalysis of Triethyl Benzyl Ammonium Chloride
    Ma Guizi, Li Ming, Yang Shiying
    1985, 6(1):  59-60. 
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    Triethyl benzyl ammonium chloride was used as the phase transfer catalyst in the preparation of diazomethane from chloform, hydrazine and sodium hydroxide. By this method the use of carcinogenic N-nitroso compound as the starting material was avoidable, and the yield were over 60%.
    Survey of the Superiority of Homologous Retention Index as a GC Characterization Parameter of Fatty Acids
    Luo Xu, Wang Xi, Cheng Lifang
    1985, 6(1):  61-63. 
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    We define homologous retention index Ih as a retention index obtained by using the homologous series of the substance to be characterized by GCas reference standards. Based on the analysis of hierarchial data with five sources of variation, we have come to the conclusion that the relative standard diviations of the proposed homologous retention index caused by the factors of concentration of stationary phase and column temperature are much smaller than those of relative retention and Kovats retention index. Therefore homologous retention index is most precise, and can be used more reliably for characterization purposes, and is expected to find broader applicability. Kovats retention index may be looked on as a special case of homologous retention index when applied to paraffin hydrocarbons.
    Structure Determination of Some Heptanedinitrile and Heptanedioic Acid Derivatives by Using NMR Technique
    Zhao Chengzhi, Ren Zhongjiao, Li Ying, Huang Huamin
    1985, 6(1):  64-68. 
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    13C-NMRand 1H-NMRspectra of 13 heptanedinitrile and heptane-dioic acid derivatives have been determined. The structures of these compounds are reported in this paper.The ordinary APTmethod was improved by combining APTwith OFR, so that both APTand OFReffects can be observed in a single experiment now.
    Crystal Structure Research of Complex K4Na2{Cu[C(CH3)(OH)(PO3)2]2}·12H2O
    Pan Zuohua, Jin Xianlin, Shao Meicheng, Zhuang Ruifang, Xiao Yongzhuang
    1985, 6(1):  69-73. 
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    This thesis reports crystal structure of the complex, K4Na3{Cu[C-(CH)5(OH)(PO5)2]2}·12H2O. The structure was determined by Patterson method and refined by block least squares routine.The final deviation factor is:R= 0.0413.Title compound crystallizes in space group P1 with crystall-ographic parameters a=ll.951(3), b = 6.220(1), c = 11. 789(2)Å; α=113.166 (11)°β= 108.944(15)° γ = 97.563(14)°;V = 727.4Å5; Dc = 2.02g/cmÅ3 and μ(MoKa) = 16.9cm-1.The result of crystal structure, analysis shows that the copper atom in each chelate ion is coordinated by four oxygen atoms of phosphoryt groups and two oxygen atoms of hydroxyl groups.
    A Theoretical Calculation of the Hydrogen Evolution Reaction Velocity at the Mercury Electrode
    ZhangLinshao
    1985, 6(1):  74-78. 
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    The theoretically derived expressions of the current density, the height and width of the potential barrier are presented based on the thermal activation model and Schottky effect.The calculated results show that the height and width of the potential barrier decrease with increasing over-potential. It follows that the rate of successful electron transfers does not only depend on the number of particles on the solution side of the metal-solution interface which exist in appropriate quantum states but also on the height and width of the potential barrier.
    Thermodynamics of Muiticomponent electrolyte Solutions(Ⅰ)——Activity Coefficient for the System HCl+ NiCl2+H2O at 298.15K
    Liang Chunyu, Yang Jiazhen, Chu Mingchen, Yang Yongzhen
    1985, 6(1):  79-81. 
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    Activity coefficient for HCl in the system HCl+ NiCl2 + H2Owith constant total ionic strengths have been measured at 298.15Kby the EMFmethod. Treated by using Har-ned's and Pitzer's equations for the mixed electrolyte solutions the results showed that the coefficient obeys Harned's Rule in the mentioned condition above. The mixing parameters 0 and ψ in Pitzer's equation have been obtained by using three methods and the activity coeffcients for the salt NiCl2 derived from them are in agreement with each other within expcrement error.
    A Study on the "Pseudo-gel" Formation in the Preparation of Hydroxyl-Terminated Polybutadiene (Ⅰ)
    Jin Guantai, Li Tianhu
    1985, 6(1):  82-86. 
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    This article concerns primarily the phenomenon of "pseudo-gel" produced during the process of the preparation of hydroxyl-terminated poly-butadiene by anionic polymerization of butadiene monomer, using naphthalene-lithium as initiator, extract oil as solvent, and ethylene oxide as terminator. Astructural model of "pseudo-gel" was first proposed by the authors. The necessary conditions of the formation of "pseudo-gel" were discussed theoretically, Acorresponding empirical equation was also developed.
    Molecular Weight Determination of Ring Shaped Polystyrene by Viscosimetry and Ultracentrif age Sedimentation
    Huang Jiaxian, Wang Linfu, Li Chunrong, He Binglin
    1985, 6(1):  87-90. 
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    The correlation equations [η] = Kη·Ma and S0=KS·Mu for ring shaped polystyrene in toluene at 25℃ have been identified by light scattering, viscosimetry and ultracentrifugation.
    Studies on the Charge Transfer Polymerization——The Photopolymerization of Acrylonitrile Initiated by Phenothiazine
    Cao Weixiao, Shu Xiaoping, Feng Xinde
    1985, 6(1):  91-95. 
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    The photopolymerization of acrylonitrile (AN) initiated by phenothia-zine (PTZ) has been studied. The kinetic equation was determined to be Rp =Rp=K[AN]1.47[PTZ]0.41 and the activation energy of polymerization (Ea) is 7.1 Kcal/mol. Through the fluorescence spectra studies, the exciplex formation between the excited PTZand ANmonomer and an initiation mechanism involving its decomposition have been proposed.
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