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    24 April 1988, Volume 9 Issue 4
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    Articles
    Synthesis and Characterization of Some Metal Complexes of Morpholinobiguanide
    Guan Yintong, Wang Yijun, Meng Qingjin, Tang Wenxia
    1988, 9(4):  311-316. 
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    Thirteen new metal ion complexes with morpholinobiguanide (formula C6H13N6O) have been synthesized, and characterized by elemental analysis,molar conductivity,TG-DTAand UVspectrum.The electronic paramagnetic resonance studies of the Cu(Ⅱ) coordination compounds with morpholinobiguanide have been carried out both in powder form and in solution. The parameters of the EPRspectra, recorded at room temperature and at 110Kin solution, enabled calculation of the covalence degree of σ and ρ bonds of the Cu(Ⅱ) ion with the nitrogen atoms of the ligand. It has been found that the a bond shows a moderate covalent nature, while theπ bond has a strong covalent character. The Mdssbauer spectra study of ferric complex with morpholinobiguanide shows that the ferric atom is in trivalent state.
    Studies on Bis-Crown Ether (Ⅳ)——Extraction of Alkali Metal Picrates with Schiff-base and Secondary Amine Type Bis-Crown Ethers Containing Benzo 15-Crown-5 Moiety
    Wang Defen, Wang Dengjin, Du Henghua, Sun Xiaoqiang, Hu Hongwen
    1988, 9(4):  317-322. 
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    Extraction of alkali metal picrates with Schiff base and secondary amine type bis-crown ethers containing benzo l5-crown-5 moiety was carried out in the medium of chloroform as water immiscible solvent. The compositions of the complexes were determined indirectly by measuring the conductance of acetone solutions of alkali metal tetraphenyl borate-crown ether. It showed that these bis-crown ethers probably formed 2:1 complexes with K+, Rb+, Cs+. The distribution ratio,extraction equilibrium constants Ke were also measured. The Ke dataindicated that for the same alkali metal picrate, the Schiff-base type bis-crown ethers give smaller values than the secondary amines. The secondary amine typebis-crown ether F2 exhibited the greatest effectiveness of extraction and selectivityfor potassium ions.
    Zero-current Oscillo-bipotentiometric Titration on Two Ag-TPB Electrodes
    Bu Haizi, Gao Hong(H. Kao)
    1988, 9(4):  323-327. 
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    Silver tetraphenylborate(Ag-TPB) electrodes were prepared by successive soaking of silver plate (or graphite rod or platinum plate) in separate 0.05 rnol/Laqueous-solutions of Na-TPBand AgNO3 for 0.5 hour.The plate or rod was then-washed thoroughly with distilled water untill free from silver ions. Such electrodes can be-used as indicator electrodes for bipotentiometric titration of Na-TPB with AgNO3. The sudden change of potential difference(AE) between two indicator electrodes at the end point was observed with an oscillograph. The method has remarkable advantages over the ordinary bipotentiometric method and can be used in medicine analysis.
    The Application of Atomic Absorption Spectrometry to Organic Analysis (Ⅰ)--Determination of Total Amount of Thiogluocosides in Rapeseed
    Tian Liqing. Wang Jide, Wang Liansheng, Ye Changling
    1988, 9(4):  328-332. 
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    On the basis of the reaction of sulfate with standard barium in water solution, an indirect method for the determination of total amount of thioglucosides in rapeseed by Zeeman AAShas been developed.The operating conditions are as following, wavelength 553.6 nm, lamp curent 10mA, silt width 1.3 nm, burner height 7 mm, flow rate of air and acetylene 9.4 L/min and 2.5 L/min, respectively.The method can be outlined as follows:a known weight sample of rapeseed is placed in a constant temperature bath(55℃)for an hour, after enzymolysis, put it into boiling water for 5 min, remove residure by filtration, dilute the filtrate to a definite volume, take a suitable aliquot of the filtrate to a calibrated centrifuge tube, add a given amount of barium, place the tube in boiling water for 5 min, cool, dilute to mark, mix, determine the excess barium by AAS.Rapeseed sample containing different amount of thiogluoosides from 35.9 to 98.2 μmol/g are analyzed, the standard deviations are 2.72 to 7.83 μmol/g, coefficients of variation are 0.0354 to 0.174, and the method is compared with volumetric analysis, the results obtained are satisfactory, the regression equation is Y = 12.836 + 0.7838X the correlation coefficient is 0.935.
    Simplex Optimization of HPLC to Separate and Determine Vitamin E Isomers
    Deng Bo, Chen Pejrong, Cai Xiaojia
    1988, 9(4):  333-336. 
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    The paper describes HPLCmethod for the determination of α-, β-,γ-,δ-isomers of Vitamin Ein by-products of refined plant oil. Asimplex method wasadopted to optimize the chromatographic conditions and a practical program was worked out. The experimental results are acceptable and the simplex method is proved to be very useful for selection of conditions in HPLC.
    The Theoretical Analysis of Interferences of Overlap Bands in Derivative Spectrophotometry and Its Application
    Li Jianjun, Luo Qingyao, Zeng Yun'e
    1988, 9(4):  337-341. 
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    This paper, from the quantitative angle, discusses the interferences, of overlap bands with each other in derivative spectrophotometry. Some theoretical criteria and formulas of error were obtained and demonstrated by the experimental data. By means of theoretical analysis, we selected the third derivative spectra for the determination of uranium (Ⅵ). The interference of Th is limited. The maximum relative error is 11%.
    Syntheses and 1HNMR Spectra of Aikenyicyclopentadienyl Ⅳ B Group Metal Derivatives
    Chen Shoushan
    1988, 9(4):  342-347. 
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    6,6-Dialkylfulvene reacts with allyl Grignard reagents to give addition products 1,1-dialkyl-3-butenylcyclopentadienyl magnesium chloride or bromide .When phenylacetylenic sodium is used instead of the Grignard reagent, the substituted fulvene forms substituted vinylcydopentadienyl sodium through a double bond shift. These substituted cyclopentadienyl anions react with metal chlorides of Ⅳ Bgroup to form a series of novel substituted metallocenes.
    Preface
    Synthesis of Derivatives of Methyl 3-(P-Amino-P-Ethoxyphosphinoyl)Propanoate
    Chen Ruyu, Liu Zhun, Liu Ziping
    1988, 9(4):  348-352. 
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    Fourteen new compounds with the general formula EtOP (O)(NHR')CH2—CHRCO2Me(R = H, CH3; R'=H, i-C3H7, n-C3H7, n-C4H9, Ph,PhCH2, p-BrC6H4, p -MeC6H4,o-MeC6H4, 3,4-Cl2C6H3, PhNH,CH2CH2OGH2—CH2*)haye been prepared by the reaction of methyl chlorophosphinoylpropanoate with various amines and identified by means of elemental analysis, lR and 1H NMR.Results from the preliminary biological tests showed that some of the compounds have weak inhibitory effects to the growth of barnyard grass, but increased the weight of rape significantly.
    Articles
    Studies on Polypeptides (Ⅳ)——The Study on Fragments of Alpha-Human Atrial Natriuretic Polypeptide
    Liang Weisheng, Peng Shiqi, Cai Mengshen, Cheng Tieming, Zhang Jingli, Dai Dunhua, Zhong Mingnai, Li Jinxiang, Chen Jisheng, J. K. Chang
    1988, 9(4):  353-357. 
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    In this work the structure of fragments of alpha-human atrial natriuretic polypeptide was determined by fast atom bombardment mass spectrometry. By analysing the m/z values of the fragment ions the sequences of amino acids can be expressed clearly. In molecular area all of the ione-are [M+H]>+ ions. The mass of C-terminal fragment ion is exactly the fragment mass, but the mass of N-terminal fragment ion is generally equal to the mass of the fragment pit's two hydrogen atoms.
    Mathematical Modeling of Hydrogen Permeation in Electroplating
    Wu Huihuang, Zhou Shaomin
    1988, 9(4):  358-362. 
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    Anew mathematical model is presented for hydrogen permeation in electroplating. The equations for the permeation-current transients are derived, and used to illustrate the observations in the literature. The traditional classification of the permeation-current curves and the determination of physical parameters are discussed.
    On the Rotational Invariance of the INDO Method Including f Orbitals into the Basis Set
    Ren Jingqing, Xu Guangxian
    1988, 9(4):  363-368. 
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    In order to ensure the rotational invariancc of the onc-conter-two-eleclrcn integrals in the INDOmethod including f orbilais info the basis ECin our previous paper, we have proposed two methods to meet this requirement in the present investigation. The first one is to use the weighted average values Jμμ′,Kμμ′, and J′μμ= Jμμ′+2Kμμ′ for the integrals (μμ| vv), (μV,μV) and (μμ|μμ), respectively. The second is a more stringent alternative, in which we have derived 690 nonzero hybrid one-center-two-electron integrals in addition to coulomb and exchange types as expressions of Slater-Condon parameters.
    A Study of UV Spectra of Me-(SiMe2)-nMe with σ→σ* Transitions
    Li Zhiru, Sun Chiachung
    1988, 9(4):  369-373. 
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    The UV Spectra of Me-(SiMe2)-nMe with n = 2,3,4,5,6 have been analyzed by means of the EHMO-CI-SPIN-FREEmethod with four-orbital model. The first and second absorptoin bands arise in essence from the σ→σ* transitions. Furthermore, the contributions of d atomic orbitals in σ and σ* molecular orbitals are discussed in detail.
    A Study on Salt Effect of Vapour-Liquid Phase Equilibrium in the Formic Acid-Acetic Acid-Water-Calcium Chloride System
    Li Xi, Jiang Fuming, Kang Hongye, Lou Ruyi, Xiu Qintang, Fan Shuguang
    1988, 9(4):  374-377. 
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    Vapour-Liquid equilibrium was measured by Otsuki-Williams still at 98658.28Pa. Analyses were made of the 3-component system AcOH-HCO2H-H2O and the 4-component system AcOH-HCO2H-H2O-CaCl2 at the vapour-liquid equilibrium.CaCl2 was used 0.5 mol/(kg solv).The results show that the favorable effect of CaCl2 is physical chemistry action.It related to the phenomena of salting-out and salting-in.
    A Study on the Conductance of KBr, KSCN, and KClO4 in DMF and Its Mixture with 1,4-Dioxane
    Zhang Hong, Liu Ruilin, Li Zhifen
    1988, 9(4):  378-383. 
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    The transport property of electrolyte solution involves the information about ionic solvation and association of ion pairing. The measurement of conductance is one of the basic methods for study on electrolyte solution. Authors have measured the variation of conductance of KBr, KSCNand KCIO4 with concentration of salt at various composition of mixed solvent of DMF with 1,4-dioxane. The viscosity of solvent and the density of the salt -solution have been determined too. According to the conductance equations, namely Pitts equation (P), Fuoss. 1978 equation (F-78), and Lee-Wheaton equation (L-W), combined with ionic association equilibrium and Debye-Huckel equation for ionic mean activity coefficient, the experimental data were fitted on IMS-8000 computer to get the parameters of theoretical conductance equations, A0, limit molar conductivity of salt at infinite dilution, Kα, ionic association constant and R, the distance between cation and anion. The parameters and the suitability of theoretical equations for the variation of conductivity of salt in mixed solvent were discussed.
    Studies on Kinetics and Mechanism of the Anionic Equilibrium Polymerization of α-Methylstyrene Initiated by n-Butyllithium/Tetrahydrofuran
    Liang Liang, Guo Shaohua, Ying Shengkang
    1988, 9(4):  384-388. 
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    The kinetics of anionic equilibrium polymerization of α-methylstyrene in the cyclohexane solution, with n-butyllithium as an initiator and tetrahydrofuran as an additive, was investigated. In the present paper.the reactive species in the system are discussed and the mechanism of polymerization is postulated. The relationships of equilibrium monomer concentration with respact to the rate constants of reactive species and the concentration of additive are obtained at 20℃.
    The Propagation Mechanism of 8,9-Benzo-2-Methyl-ene-1,4,6-Trioxaspiro[4,4] Nonane
    Pan Caiyuan, Lü Shaoxiang
    1988, 9(4):  389-393. 
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    Based on the possible propagation reaction of 8,9-benzo-2-methylene-1, 4,6-trioxaspiro [4,4] nonane (Ⅰ), initiated by free radical initiators, a kinetic equation has been deduced. The rates of monomer(Ⅰ) Consumption and phthalide formation during the polymerization were measured by IRand the experimental results confirmed the kinetic equation. This demonstrates that the propagation reactions of monomer (Ⅰ) include two reactions addition polymerization and ring-opening -isomerization-addition polymerization. The relative contribution of these two reactions to the total polymerization rate depends on the monomer concentrations. The structure of polymer is measured.
    Studies on the Tetranitrato-Bis(4,4'-Dimethyl-2,2'-Bipyridine)Cerium (Ⅳ) and Tetrachloro-Bis (4,4'-Dimethyl-2,2' -Bipyridine Hydrogen Chloride)Cerium(Ⅳ)
    Zhu Wenxiang, Ren Yingjie, Zhao lizhou
    1988, 9(4):  394-397. 
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    Two title complexes were isolated. Spectroscopy studies show there is a similarity between the two complexes. The NMRspectrum suggests that the two nitrogen atoms in complex CeCl4(dmbipyHCl)2 are chemically non-equivalent. It may reveal the coordination of a nitrogen atom of bipyridine in that complex to the central ion.
    Synthesis and Characterization of Solid Fluorescent Complexes of 1,8-Naphthyridine-N-oxide with Alkaline Earth Nitrates
    Gan Xinmin, An Yonglin, Tan Minyu
    1988, 9(4):  398-400. 
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    The solid fluorescent complexes of 1,8-naphthyridine-N-oxide with alkaline earth nitrates have been synthesized. The new complexes have the composition M(napyo)a(NO3), (M = Mg, Ca, Sr) and Ba (napyo)2(NO3),·H2O determined by elemental analyses. Their solubilities in various solvents and molar conductance in methanol have been determined. The 1Rspectra show that the oxygen atoms in 1,8-naphthyridine-N-oxide are coordinated to the metal ions of alkaline earth. The fluorescence spectra indicate that the fluorescence intensity of the complexes decreases successively from Mg to Ba. The DTA-TGdata show that the complexes are all relatively thermally stable.
    Study on Response Equation of Non-Nerrist Range of Ion-Selective Electrode——Application of PVC-AD Electrode in Low Concentration Range
    He Xinghai, He Yarning, Deng Bingyan, Hua Huizhen
    1988, 9(4):  401-403. 
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    In this paper "a new response equation of Non-Nernst range of electrodes is derived and a quantitative analysis method is established. This method makes the electrode to be used to measure content of anionic surfactant in drinking water and surface water. The results show that the method would replace methylene blue colorimetric method.
    Simultaneously Spectrophotometric Analysis of Multicomponent Systems——Nonlinear Equation Set Method
    Ni Yongnian
    1988, 9(4):  404-406. 
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    Anonlinear equation set method for simultaneous determination of multicom-ponent systems is presented. The method was applied to the inorganic colored systems which severely deviate from the Beer's law. The data processing was carried out by matrix calculation.Two-demonstrations of ..determination with this method are given and their results are satisfactory.
    Spectrophotometric Study of the Reaction of Fe(Ⅱ) with 2-(2'-Benzothiazolylazo)pyrocatechol
    Feng Jianzhang, Li Yan
    1988, 9(4):  407-409. 
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    The properties of 2-(2' -Benzothiazolylazo)-pyrocatechol and its complex formation reaction with Fe(Ⅱ) were studied. Asimple and highly sensitive . spectrophotome-tric method for the determination of trace amounts of iron has been developed. Optimum conditions for the determination, linear range and the interference of various foreign ions are reported. The composition, the molar absorptivity and stability constant of MR3 were also determined. The method has been applied to the determination of trace iron with satisfactory results.
    Study on 29SiNMR of 2,2,3-Trihydrocarbylphenyl-benzo-1-oxa-3-aza-2-silacyclohexen-4-one
    Wang Mingde, Zhang Diankun, Li Guowei, Xie Qinglan
    1988, 9(4):  410-412. 
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    The 29SiNMRof 2,2,3-trihydrocarbyl phenylbenzo-l-oxa-3-aza-2-silacyclo-hexen-4-one was systematically discussed. The relationship between the chemical shifts and their molecular structure was found and explained.
    Catalytic Behavior of Ti-ZSM-5 in the Cracking of n-pentadeeane
    Jiang Dazhen. Jiang Yulin, Liu Ziyang
    1988, 9(4):  413-415. 
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    The cracking of n-pentadecane on Ti-ZSM-5 arid ZSM-5 has been measured. Cracking activities have been found to be strogly dependent on the Si/Ti ratio inthe zeolite.Titanium introduced into the framework of ZSM-5 increases the selectivity of C6~C10 formed in the cracking of n-pentadecane on the Ti-ZSM-5 during activity decay.
    Spectroscopy of Hematppqrphyrin Derivative
    Wang Yutian, Xu Weiqing, Liu Juzheng, Liang Yingqiu
    1988, 9(4):  416-418. 
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    Surface enhanced resonance Raman spectra of hematoporphyrin derivative ad-sorbed on a silver electrode were observed, and it is belived the band intensities of SERRSare three oders stronger then those of resonance Raman spectra. By means of SERRStechnique, it is expected to obtain more informative charact eristics even in dilute solution (10-5mol/L) of HpD.Assignments of some.SERRS band, of the compound have been made, and it is considered that "chemical effect" is apparent in the SERRSof HpD.
    A Study of the Catalysts in Oxidative Coupling of Methane
    Liu Qin
    1988, 9(4):  419-421. 
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    The activity, selectivity and life time of alkali metal salt catalysts carried on the surface of samarium oxide and on that of other metalic oxides used in oxida-tive coupling of methane are reported here. Meanwhile, the influence of temperature, partial pressure of methane and molar ratio of methane to oxygen on the activity and selectivity of the catalysts are determined. The results of experiments show that the most important ones are lithium chloride carried on nickel oxide and manganese dioxide. They can directly convert methane to ethylene. The output of ethylene increase to 26% and 28%.
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