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Table of Content

    24 July 1990, Volume 11 Issue 7
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    Articles
    Studies on the Solid State Reaction of Coordination Compounds (XXVI) ——Solid State Synthesis and Crystal Structure of Compound WS4Cu3(PPh2)3Cl
    Liu Shixiong, Huang Jinling, Gao Fengjun, Zhu Huizhen, Xin Xinquan
    1990, 11(7):  667-671. 
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    Abrown-red solid was synthesized through a solid state reaction among (NH4)2WS4, CuCl and PPh3. The solid was extracted with CH2Cl2 and then diffused with CH3OH to obtain a yellow singlecrystal WS4Cu3(PPh3)3Cl. The crystal is triclinic with a = 13. 049(3) Å, b = 20. 351(4) Å, c =11. 876(2) Å, a=94.75(2)°, β=115. 97(1)°, γ=74. 90(2)°, space group P1, z=2. The titlecompound molecule has a cluster core Cu3WS3Cl. The average distance of W- Cu is 2. 719Å.
    Studies on Bis-Crown Ether ( V )——Extractive Behaviour of Alkali Metal Picrates with Schiff Base and Secondary Amine Type Bis-Crown Ethers Containing Benzo-18-Crown-6 Moiety
    Wang Dengjin, Wang Defen, Sun Xiaoqiang, Hu Hongwen
    1990, 11(7):  672-675. 
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    Extraction of alkali metal picrates with two different kinds of schiff base and secondary amine type bis-crown ethers containing benzo-18-crown-6 moiety was carried out in chloroform at 25 ±0. 2℃. The distribution ratio of alkali metal picrates, the stoichiometry and extraction equilibrium constants Ke of bis-crown ether-cation complexes were determined. The results show that the bis-crown ethers form 1 : 1(crown unit : cation) cpmlexes with Na+,K+,Rb+ and probably form 2 : 1 intramolecular or intermolecuiar complexes -with Cs+, but mono Schiff base type bis-crown ethers preferably form 1 :1 complexes with Cs+. Moreover the Ke, values of the secondary amine type bis-crown ethers are much larger than those of the Schiff base type bis-crown ethers. N1 exhibits the greatest extractibility and selectivity for Cs+ ions. It is noteworthy that the bis-crown ethers N5 containing unsymmetrical crown rings has a larger extractibility for Rb+ ions.
    A Study on Synthesis and Structure of S APO-11 Silicoaluminophosphate Molecular Sieves of SAPO-11 Type
    Xu Yihua, Hu Qifu, Lu Yuqin, Xu Ruren, Ma Heyuan
    1990, 11(7):  676-680. 
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    SAPO-11 Silicoaluminophosphate molecular sieves were synthesized in a hydrothermal system with an organic agent(di-n- or iso-propylamine). There are three method: (1)The aluminum source is aluminum isopropoxide. (2)An aluminophosphate solution was used in the reactive mixture. (3) The reactive mixture includes the fluo-anions. The framework structure and pore structure of SAPO-11 were studied by means of 2nd derivative IR, XRDand sorption in a vacuum. The conditions of synthesis of SAPO-11 were discussed.
    Syntheses and Characterization of Imidazolate Bridged Heteropolynuclear Complexes Containing Zn
    Chen Dong, Tang Wenxia, Dai Anbang
    1990, 11(7):  681-684. 
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    Five species of imidazolate bridged heteropolynuclear complexes containing Zn ( Ⅱ ) were prepared. In the syntheses, the kinetically inert, low spin d6 complexes, [(NH3)5CoIm]2+, [(NH3)5RhIm]2+ and [(en)2Co(Im)2]+ were used as ligands to react with mononuclear Zn ( Ⅱ ) complexes. By elemental analysis, molar conductivity, TGA, DSC and 1H NMR study, all bridged heteropolynuclear complexes were characterized.
    Subtraction of Background Current in Polarographic Curves
    Tian Baoming, Chen Hongyuan, Xiao Zhaohua
    1990, 11(7):  685-688. 
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    A accurate, reliable method for correcting the background current in polarographic curves with digital computer has been developed. In this method, the fitting function proposed is composed of the multinomial B(E) =a/E + b + cE + dE2, as a background function, and the polarographic peak function which is obtained by the combination of polarographic peak-current equation with revised Guassian function.By employing the nonlinear least square parameter estimation from the experimental curves, the Faradaic peak currents, peak potential and width of half-peak can be calculated without the need of the data of blank solution. This method has been applied to ACPand DPPfor subtracting the background current with satisfactory results.
    Studies on Chelate Reaction of New Fluorescent Reagent SPAEC with Gallium (Ⅲ) and Its Analytical Application
    Li Zhiliang, Yu Ruqin
    1990, 11(7):  689-692. 
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    Anew fluorescent analytical reagent 2-(5'-sulfo-2'-hydroxyl-1'-phenylazo)-5-ethy-lamino-4-cresol(SPAEC), which has been synthesized recently in our laboratory, was applied to the fluorimetric determination of gallium. The optimal conditions for fluorescent complex formation of SPAECwith gallium ( M ) were established. At pH 3. 8-5. 5, a 1 : 1 type complex was formed with λex/λem of 515/585 nm and with quantum yield (φF) of 0. 046. The proposed method was used for the determination of 2 × 10-7～2 × 10-6 mol/Lgallium in semiconductor and alloy samples with good results.
    The Linear Combination of Spectrophotometry of Multi-Wavelength Data and Its Applications
    Li Menglong, Shi Leming, Liu Shuqiong, Li Zhiliang, Yu Ruqin
    1990, 11(7):  693-697. 
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    The linear combination of multi-wavelength data (absorbance) is developed as a new computational spectrophotometry to improve the selectivity and accuracy, based on the combination of simultaneous equations with a set of proper coefficients. The absorbance obtained is in proportion to the concentration of the analyzed compounds and independent of the interferents, thus the in terference can be removed. The proposed method, which has the advantage for determining multi-wavelength data with simpler computation and can be used in single or simultaneous measurement, has been applied to the analysis of compound pharmaceutical preparations.
    The Application of Capillary Flow Cell to Photoacoustic Detection
    Zuo Boli, Deng Yanzhuo, Zeng Yun'e
    1990, 11(7):  698-701. 
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    The design and application of capillary flow cell optimized for laser induced photoacoustic spectroscopic detection of effluent are described. The characteristics arid analytical figures of merit of the flow cell are presented. Application of the flow cell to the detection of Co2+ effluent is demonstrated. The detection limit of Co2+ corresponds to 2×10-6 cm-1 in absorptivity for LIPAS detection.
    Determination of Crystal Structure of Schisandrone
    Hua Suming, Wang Qiguang, Yue Jianmin, Chen Yaozu
    1990, 11(7):  702-705. 
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    The needle crystal of Schisandrone, C21H24O5, which is colorless and transparent, belongs to triclinic system. The unit cell parameters are a=9. 109(3), 6 = 9. 749(2), c= 11. 663(1) Å; α = 65.21(1), β=89. 82(1), γ=89. 96(2)(°); Z=2.In all the calculations of structure analysis, Direct Method programme of MULT AN 82 was used. All of the atomic coordinates and thermal parameters have been refined to R=0. 060 for 3521 reflections having I>3. Oσ(I). The diffractometry result shows that Schisandrone is a 4-aryltetralone lig-nan, which is the same as the result of spectroscopic determination.
    Preface
    Studies on N-Alkyl-N'-Phenylsulfonyl-N'-Ethoxycarbonylmethyl-O-Ethylphosphorodiamidoates
    Chen Ruyu, Wang Huilin, Lai Pengxiang
    1990, 11(7):  706-709. 
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    The method for the synthesis of ten new phosphorodiamidoates with a general formula: EtO(R1,R2N)P(O)N(CH2CO2Et)SO2C6H4X ( I ), (where R1,R2 = Hand lower alkyl groups, X = Me, halogen and nitro groups) is described. The structures of ( I ) were confirmed by 1H NMR and elemental analysis, A one-pot reaction was investigated; the preliminary bioassay shows.that some of these new compounds have a remarkable inhibitory effect on leaf-rust of wheat.
    Articles
    Investigation on the Rare Earth Complexes of 2-Hydroxy-3-p-Bromophenyl-Maleimide
    Yang Dilun, Zhu Yu, Liu Youcheng, Kong Suling
    1990, 11(7):  710-714. 
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    2-Hydroxy-3-p-bromophenyl-maleimide (HBPMI) has two acidic functional sites including the ring nitrogen atom and the 3-hydroxy group. Thirteen rare earth metal complexes were prepared by the reactions of HBPMIsodium salt with RECl3 in DMSO under Ar atmosphere. There complexes were studied by means of IR, UV, 1H NMR, 13C NMR and elemental analysis. The results indicate that it is the deprotonated hydroxy group of the HBPMIthat bonds with RE3+, but not the nitrogen. Participation of the adjacent carbonyl in coordination was not found. The composition of the complexes is RECl3. nH2O(RE=La-Lu, except Pm, Yb; Lis the HBPMI-oxide anion, n=2～4). RE-O bond is considered to be ionic with some degrees of covalent character. The shift rule of the RE-O bond strength does not conform the rule of tetrad effect. It was found that the conjugation between p-bromophenyl and maleimide moiety in the HBPMI-oxide anion of the rare earth complexes is stronger than in the HBPMIitself, and that the charge is transferred from the negative oxygen to the p-bro-mophenyl moiety.
    A Quantum Chemical Study of Chemical lonization of N-Nitrosodimethylamine (NDMA )
    Guo Chunxiao, Meng Qingbo, Liu Shuying
    1990, 11(7):  715-719. 
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    In this paper the structure and properties of N-nitrosodimethylamine(NDMA) were studied by means of chemical ionization mass spectrometry(CIMS) and quantum chemical calculation. The protonated dimer ion of NDMAis observed and the geometries of the corresponding ions are optimized by using CNDO/2 method in the CIMS. The forming pathway and broken bond mechanism of protonated ions were explained theoretically. We have also analyzed the electrostatic potentials of NDMAand (NDMA)H+ as well as tried to explain the carcinogenic machanicm.
    Pressure Effect of Raman Active Modes of Melamine and Induced Phase Transition by Pressure
    Zhao Yongnian, Zhang Zhaojin, Cui Qiliang, Liu Zhenxian, Li Dongmei, Zou Guangtian
    1990, 11(7):  720-724. 
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    High-Pressure Raman spectra for C3N6H6(Melamine) were measured at the range of 0～8. 7 GPa. The pressure effect of the intensity, frequency and mode-Gruneisen parameter(vi) were discussed. The Experemental results show that melamine probably undergoes two structural transitions at 2 GPa( Ⅱ ) and 6 GPa( Ⅲ ) respectively and phase Iis of Ci ymmetry probably.
    Effect of Micro-Sodium on Solidification Process of Al-Si Eutectic Alloys
    Wang Zichen, Wang Xiaohui, Zhang Lihua, Shong Lizhu, Zhao Muyu
    1990, 11(7):  725-728. 
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    The influence of micro Na on the solidification process of Al-Si alloys was investigated by differential thermal analysis. It is found that the addition of micro Na raises the eutectic nucleation temperature and retards the eutectic crystallization of the melted Al-Si alloys, which is contrary to the traditional view point.
    The Effect of Additives on the Performance of Anodically Deposited Lead Dioxide Electrode
    Zhou Yuanquan, Zhou Yunhong, Gao Rong
    1990, 11(7):  729-732. 
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    The effect of the additives, which were added in the solution for preparing the PbO2 anode, on the performance of the anodic ozone evolution on the PbO2 electrode has been studied. The results show that halide and transition metal ions have an influence on the performance and morphology of deposited PbO2 film on the iron electrode. The activity and stability of the PbO2 anode for ozone evolution were significantly improved, when both chloride ion and ferric ion were used as the additives. A nonporous lead dioxide film on the iron plate has been thus prepared.
    Permeation and Entrainment Swelling in W/O/W Emulsions
    Yan Nianxi, Shi Yajun, Su Yuanfu
    1990, 11(7):  733-738. 
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    The permeation and entrainment swelling in W/O/W emulsions were studied in the batch stirrers experimentally. The results show that the permeation swelling increases with increasing the osmotic pressure difference between the internal and the external phases as well as the concentration of the surfactants and the carriers in the membranes, but decreases with increasing the membrane viscosity. When the osmotic pressure difference is higher, the effect of the water permeation on swelling is larger than that of the entrainment. The effect of the oxygen-containing compounds in the membranes on swelling is larger than that of the nitrogen-containing compounds. When span 80 was used as the surfactant, the permeation swelling was 6 times higher than when E644 was used, and the entrainment swelling was also higher. Repeated of coalescence and redispersion can promote the swelling caused by the entrainment. From these results, it is concluded that the multistage mixer-settler seems unsuitable to the liquid membrane, operations.
    Studies on the Synthesis and Chromatography Properties of Copolymers Crosslinked with Triallyl Isocyanurate
    He Binglin, Guo Xianquan, Yang Zhixin,Zhao Fengzhi, Yu Zhanru
    1990, 11(7):  739-742. 
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    The copolymer were synthesized from vinyl acetate and triallyl isocyanurate under conventional conditions. Their specific surface area, average pore radius, pore volume and swelling capacity were determined. At the same time the copolymers were used as a stationary phase for gas chromatog-raphy and the column effeciency, peak symmetry and separating size were investigated. They can be used for rapid separation of a few mixtures which are separated difficultly, we expect that they will be used wildely.
    Situdies on Sulfonated Polyurethane Anionomers ( I ) ——The Effect of Different lonization Levels on their Properties
    Zhai Honglian, Yu Xuehai, Yang Changzheng
    1990, 11(7):  743-747. 
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    The sulfonated polyurethane anionomers were synthesized by the ionization of polyurethane, which was prepared by using polytetramethylene oxide (PTMO) as the soft segment and 4,4'-diphenylmethane diisocyanate (MDI) and 1,4-butanediol(BD) as the hard segment, with sodium hydride and r-propane sultone. Their properties were investigated by using IR, differential scanning calorimetry, dynamic mechanical analysis and stress-strain testing. The results indicate that the compatibility of soft segment and hard segment varies with the degrees of ionization. Introducing a small amount of ionic group results in an increase of compatibility of soft and hard segments, but further ionization can increase the degree of phase separation. The mechanical strength and hydrophilicity are gradually increased with the increase of ion content. A new approach for controlling the hydrophilicity of polyurethane and preparing water soluble polyurethane was developed.
    Studies on the Polarographic Adsorptive Wave of Mercury ( Ⅱ )-Palladium Reagent Complex
    Gao Zhiqlang, Sun Yanyi, Zhao Zaofan
    1990, 11(7):  748-750. 
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    The polarographic adsorptive wave of Hg ( Ⅱ )-palladium reagent (3-hydroxy-1-p-sul-fonatophenyl-3-phenyltriazene) complex in 0. 05 mol/L Na2B4O7 medium was studied for the first time and a sensitive SSP(single sweep polarography) method for the determination of trace of Hg( Ⅱ ) has been developed. The complex, corresponding to Hg(R)2 with logβ'=8. 30, is strongly, adsorbed on the surface of the mercury electrode. The polarographic wave is attributed to the reduction of Hg ( Ⅱ ) In the complex to Hg. The linear range is from 7×10-8 to 1×10-5 mol/Land the detection limit is 4 × 10-8 mol/L. The method has been used to determine Hg(Ⅱ ) in water and biological samples.
    Studies on the Preparation and Properties of Trialkoxyl (β-Alkoxycarbonyl) ethylgermanium
    Bai Mingzhang, Yang Shujun, Sun Lijuan, Liu Hongmei
    1990, 11(7):  751-753. 
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    Fourteen new organogermanium compounds were prepared and characterized by elemental analysis, IR and 1H NMR spectra. The hydrolytic reactions of the title compounds were carried out.
    Synthesis and Reactions of 1, 1-Di-cyclopentadienyl-2,3-diphenyl-7-methyl- 1-zirconoindene
    Chen Meiwen, King Keyuan
    1990, 11(7):  754-755. 
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    By the thermolysis of di-o-tolylzirconocene and tolane, new zirconoindene complex was obtained with a high yield. The data of elemental analysis, spectra and MS were provided. The acidoly-sis and iodolysis of zirconoindene were studied, By the identifications of the products, the structure of zirconoindene was determined. Because of the high yield and selectivity in the formation and acidolysis of zirconoindene, these reactions are useful in stereo-specific organic syntheses.
    Preface
    Synthesis of 1-Acyl Benzoimidazole and 3-Acyl-2-Thiothiazolidone Derivatives
    Wang Duhu, Wang Dazuo
    1990, 11(7):  756-758. 
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    The 14 new derivatives of 1-acylbenzoimidazole and 3-acyl-2-thiothiazolidone have been prepared by the reaction, of benzoimidazole or 3-thiothiazolidone with 4-alkyl-4-cyano-4-phenyl-bu-tanoyl chloride in the presence of organic bases such as triethylamine, pyridine or benzoimidazole itself, the acyl chlorides are not purified from the reaction of the corresponding acid and thionyl chloride. It has been shown that all compounds prepared have definite fungicidal effects from the results of ten pathogens test.
    Articles
    Studies on Selective Oxidation of α,β-Unsaturated Alcohols——The Synthesis of Two New Types of Polymer Supported Oxidizing Reagents and Their Excellent Selectivity
    Yang Hulrong, Li Bina, Lu Qiansheng
    1990, 11(7):  759-761. 
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    Two new types of polymer supported oxidizing reagents——dichromic acid type tertiaryamine resin and dichromic acid type quaternary ammonium resin were synthesized by using jel tertiary amine resin and jel quaternary ammonium resin as the supports. These two new types of polymer supported oxidizing reagents can successfully oxidate the α, β-unsaturated alcohols into the corresponding α,β-unsaturated aldehydes, but can not oxidate the saturated alcohols under the similar condition, which exhibits excellent selectivity.
    Synthesis of New Ferrocene Derivatives Containing α,β-Unsaturated Ketone Group
    Zhang Chengru, Yin Yongjun, Zhou Yaokun, Wang Liufang
    1990, 11(7):  762-764. 
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    Anew method is given for the synthesis of 4-ferrocenyl-3-pentene-2-one, which involves the condensation of ferrocene with acetylacetone in concentrated sulfuric acid at -5℃. The acylation reactions of this compound is investigated, and four new derivatives are prepared. All of these compounds are identified by 1H NMR, IRand elemental analysis.
    The Influence of Inert Carrier Gasses on TPR Kinetics
    Duan Xue
    1990, 11(7):  765-767. 
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    By the study of temperature programmed reduction (TPR) for some copper oxides, it is shown that when the gasses used as inert carrier are different, there are some differences in kinetic character of the reduction reaction although other conditions are the same. In this paper, the TPRcurves of some copper oxides, obtained by using of N2 and He respectively, have been analyzed qualitatively and quantitatively. Combining the mechanism of the reduction and statisitical thermodynamics with the results metioned above, it is supposed that the main reason of this phenomenon is that the molecular diameter of different inert carrier gasses are different.
    13C NMR Studies of Humic Acids from Soils
    Dou Sen, Hua Shiying, Zhu Tao
    1990, 11(7):  768-770. 
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    The 13C NMR spectra were measured for humic acids from several cultivated soil (black, brown forest, meadow and paddy soil) in the Northeast of China. Acomparison between humic acids from peat and those from pig manure was also made. The results show that humic acids of soils mainly consist of four types of carbon: corbonyl, aromatical, alkoxy and polymethylene. Their aromaticity is less than 40%. There are some differences among various humic acids from different soils. Humic acids from peat and pig manure are characterized by lower molecular weight and lower degree of oxidation compared with soil humic acids. The aromaticity of the humic acid from peat is much higher than that from pig manure. The results also show that the 13C NMR spectrometry can be considered as one. of the most effective methods for investigating the structural characterization of humic substances.
    Infrared Photoacoustic Spectrometry Determination of Carbonaceous Material on Surface of Tungstosilicic Acid
    Wu Tonghao, Li Xia, Yang Hongmao, Wang Guojia, Jiang Yuzi, Li Yuyan, Xu Shaomin
    1990, 11(7):  771-773. 
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    FTIR-PAS was used for the structural study of carbonaceous material on the surface of tungstosilicic acid which is a catalyst for the oxidative dehydrogenation of ethylbenzene. It turns out that the carbonaceous material contains conjugated double bonds and carbonyl groups.
    Determination of Counterion Binding Degree of Micelles by Ion-selective Electrode
    Zhu Demin, Zhao Guoxi
    1990, 11(7):  774-776. 
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    An advanced method used to determine the counterion activity in micellar solution by ion-selective electrode is described, and a new equation dCcf/dCiT=-K is derived where Ccf denotes the concentration of unbound counterions, and CiT is the concentration of ionic surfactant. This equation is used to calculate the counterion binding degree(K) of micelles. K values of eight kinds of ionic micelles are investigated. They are in the range of 0. 6～0. 70.
    Studies on Salting-out Constants and Activity Coefficients of Polycyclic Aromatic Hydrocarbons in Aqueous Salt Solutions
    Wang Liansheng, Xu Liangji, Li Xiaojuan
    1990, 11(7):  777-779. 
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    The solubilities of polycyclic aromatic hydrocarbons in water as well as in the aqueous NaCl salt solution were determined at 25℃ by spectrophotometer. The activity coefficient and salting-out constants have also been calculated.The salt concentrations (Cs) used are in the range of 0～0. 8 mol . L-1 when lgf values were ploted vs. Cs for each compound, the obtained results are all straight lines. On comparison of slopes of these lines, the salting-out order is 4-methyl biphenyl>biphenyl>Naphthalene>ether>a-methyl naphthalene.
    Studies on the Atomization Mechanism of Elements on the Graphite Probe Surface in the Graphite Furnace——The Atomization Mechanism of Cadmium and Aluminium
    Deng Bo, Luo Yanfei
    1990, 11(7):  780-782. 
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    The atomization mechinism of cadmium and aluminium on the graphite probe surface in the graphite furnace is studied. The result shows that the atomization of cadmium and aluminium on the graphite probe surface originates from the thermolysis of their monooxides. The appearance temperature of Cd and Al is identical with the thermolysis temperature of their oxides respectively. The active energy of atomization is related to the bond energy of M-O of their oxide.
    Synthesis and Characterization of Poly(2,2,3,3-Tetrafluoropropyl Methacrylate) and Its Copolymers with Methyl Methacrylate
    Li Chunrong, Li Yaozhu, Xu Yueping, Song Yuexian, Zhu Duanhui, Huang Jiaxian
    1990, 11(7):  783-785. 
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    Homopolymers and copolymers of fluoroalkyl methacrylate are the important materials for plastic optical fiber. In this paper the method of the monomer synthesis and the homo- and the copoly-merization condition were reported. Polymers with high molecular weight are obtained by using this method. The theoretically calculated results of the refractive index of the polymers according to the theory of group contribution are in agreement with those of the practical measurements. The Mark-Houwink equations [η]THF25℃=3.54×10-3×M0.73, [η]Acetone25℃=2.34×10-3×M0.75 of the homopolymer are identified by measuring with light scattering and viscosity.
    The Effect of Acidity of Polymerization Medium on Structures and Properties of Polyaniline
    Su Zhixing, Liu Xiangqian, Sheng Fenling
    1990, 11(7):  786-788. 
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    In this paper, polyanilines were prepared by the chemical oxidation of aniline on different acidity conditions, their structures and properties and the relationship between them and the polymerization acidity were studied by IR, ESR, X-ray diffraction and so on. Asignificant result was obtained.
    A Study of the Molecular Weight of Xanthan
    Wang Derun, Yu Xianchao, Zhao Dajian, Cao Wuxiong, Kang Zhadwen, Wang Yi
    1990, 11(7):  789-791. 
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    The methods of ultracentrifugation, measuring molecular length by transmissive electron-microscope and small angle laser light-scattering were used to determine the molecular weight of self-made xanthan. The molecular weight measured by the three methods above are 2. 5×106, 6×106-2. 5×106 and 2. 36×106 dalton, respectively. Three results are well consistent with each other.
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