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Table of Content

    24 December 1987, Volume 8 Issue 12
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    Articles
    The Influence of Trace Amounts of Aluminium on the Crystallization of Heteroatom-Containing ZSM-5-Type Zeolites
    Feng Shouhua, Xu Ruren
    1987, 8(12):  1053-1058. 
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    The present paper reports the systematical investigation of the influence of trace amounts of aluminium on the formation and crystal growth of M-Si-ZSM-5 type zeolites(M=B,Ga,Ti,V,Cr and Fe).It is shown that a trace of aluminium plays "nucleation-assisting" role in the formation of heteroatom-containing ZSM-5 type zeolites and accelerates the crystal growth of these zeolites by means of the comparison experiments of adding Al to the system of HMDA-Na2O-MOx/2-SiO2-H2O, electron diffraction, XPSand the calculation of the crystallization kinetic model.
    Study on the Structure of AlPO4-5 Type Molecular Sieve in the Framework P and Al Substituted Equal-Proportionally by Hetero-Atom(Si)
    Meng Xianping, Pang Wenqin, Li Wangrong, Liu Zhenyi, Zhang Wanjing
    1987, 8(12):  1059-1063. 
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    The structure of Si-APO-5 type molecular sieve synthesized by us was investi-gated by X-ray diffraction for polycrystalline and the parameters were refined by Rietveld method. We discovered, although in average each unit cell 3.13 silicon atoms substituted equal-proportionally P, Al and entered framework of molecular sieve, SAPO-5 sample (10900) still keepcd the same symmetry and geometric configuration as APO-5. In addition to, the arrange of Si, P, Al in the framework were disorder on the whole, therefore, framework of molecular sieve lost polarity along[001] and cann't carry charge. So as Si atom substituted Pand Al atoms in framework equnl-proportionally, catalytic functions of APO-5 type molecular sieve cann't be outstanding adjusted.
    Synthesis and Characterization of Ni(Ⅱ)Complex with a 14-Membered Hexaaza Macrocyclic Ligand Containing Pyridine
    Liao Daizheng, Zhou Li, Wang Genglin
    1987, 8(12):  1064-1066. 
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    A new nickel(Ⅱ) thiocyanate complex containing a 14-membered hexaaza macrocyclic ligand(L), [NiL(SCN)2]·H2O, has been prepared by template condensation of 2,6-diacetylpyridine with hydrazine. Based on IR, electronic spectra, electrical; conductance, magnetic moment, thermal and elemental analyses, this complex is proposed to have six coordinate and distorted octahedron configuration.
    Studies on Co-luminescence Effect of Rare Earths(Ⅱ)--The Co-luminescence Effect of Sm-Tb TTA-Phenanthroline-System and Its Analytical Application
    Zhu Guiyun, Yang Jinghe, Ge Wen, Wang Lei
    1987, 8(12):  1067-1070. 
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    A co-luminescence effect of Sm-Tb-TTA-phenanthroline(phen) system was first studied. We observed a new fluorescence-enhanced phenomenon, which occurred by adding some of rare earths to above system. Amony them, Tb3+increases the fluorescence intensity of Sm-TTA-phen system by 2 orders of magnitude.The optium conditions to form the system are as follows: concentration of Tb3+is equal to 1-2×10-5M, and pHis 5.5-7.0. The enhancement effect can be used for the determination of ultratrace amounts of Sm3+, the detection limit is 2.5×10-11M.
    Studies On Unstirring Potentiometric Stripping Analysis with Hanging Mercury Drop Electrode
    Kuan Xiangyuan, Chou Tuanchi
    1987, 8(12):  1071-1075. 
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    Assuming that unstirring stripping prccess of the metal in the amalgam is controlled by the limited flox of the oxidant and providing that setting time is not less than 30 second, a theory of unstirring potcntiometric stripping analysis (UPSA) with hanging mercury drop elctrode(HMDE) is presented in this paper. Experimental verification is made and it was found that the experimental results arc in agreement with the theoretic conclusion, and so the theory of UPSAis successfully approached.
    Studies on Laser-Induced Fluorimetry(Ⅰ)--Determination of the Trace Terbium with EDTA-Tiron-CTMAB Fluorescent System and Optical Multichannel Analyzer
    Hu Jiming, Deng Yanzhuo, Zeng Yun'e
    1987, 8(12):  1076-1080. 
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    The sensitization and stabilization of several surfactants on Tb-EDTA-Tiron system and the effects of Laser energy on the fluorescence intesity were investigated by using dye Laser and SITvidicon Optical Multichanel Analyzer. The Tb-EDTA-Tiron-CTMAB system was adopted in the determination of the trace terbium. The proposed method show good sensitivity, selectivity and stability compared with other fluorescent methods. The trace terbium in Y2O3are directly determined without separation.
    Catalytic Titration(Ⅱ)--Titration of Metal Ions with EDTA
    Gu Zhicheng, Zhang Ping
    1987, 8(12):  1081-1084. 
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    The method for direct titration of metal ions with EDTAwas investigated. The ligand-exchange reaction Ni-Trien+Cu-EDTA→Cu-Trien+Ni-EDTA was used as indicator reaction, which can be catalyzed by trace amount of EDTA. Cu-Trien was measured spectrophotometrially at 550nm,and used as indicator substance, then the change of the reaction rate of the indicator reaction was measured. By this method, the micromole level of Cu,Ni,Zn,Pb and Ca can be determined The titration was carried out in a borax buffer solution with. pH 10.0.For Cu2+, Zn2+,Pb2+, and Ni2+, because of the conditional stability constants of their EDTAcomplexes being greater than the corresponding value of Cu-EDTA, they can catalyze the indicator reaction, therefore the titrable range is narrow. But for the metal ions such as Ca2+, whose EDTA complex's conditional stability constant is less than the corresponding value of Cu-EDTA, the titrable range is wide, because it is of no catalytic effect on the indicator reaction.
    Study on the Reaction of 1,4-Dilitho-1,2,3,4-Tetraphenyl 1,3-Butadiene with Carbon Halide (Ⅰ)--The Molecular Structure of the Product,cis,cis-1,4-Dibromo-1, 2,3,4-Tetraphenyl-1,3-Butadiene
    Huan Zhenwei, Liu Weiguo, Chen Lin, Kao Chenheng, Yao Xinkan, Wang Honggen
    1987, 8(12):  1085-1090. 
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    Cis, cis-1, 4-dibromo-1,2,3,4-tetraphenyl-1,3-butadiene is obtained from the reaction of 1, 4-dilitho-l,2,3,4-tctraphenyl-l,3-buladicnc with carbon tetrabro-mide. The molecular structure of the product is determined by the results of elementary analysis, MS, 1R, NMR and single crystal X-ray diffraction. That, the molecular structure of the product is not coplanar, is thought to be caused by the steric hindrance between the substituents.
    A Kinetic Study on The Thermal Decomposition of meso-and di-Dietnyl 2,3-Dicyano-2,3-diphenylsuccinate in Styrene
    Yang Dilun, Zhao Wenyi, Liu Youcheng
    1987, 8(12):  1091-1095. 
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    The kinetics of the thermal decomposition of rneso-(1) and dl-dieihyl-2,3-dicyano-2,3-diphenylsuccinatc(2) in styrene at different temperatures were studied by means of dilatometry. The activation parameters were found to be. Ed=93.2 + 3kJ·mol-1, △S≠=-12.7+1 eu for 1; Ed=120.8±3kJ·mol-1, △S≠= 1.8 ±1eu for 2. The conclusion is that the dl-isomer is more stable than the meso-isomer on the basis of the rate constant for the decompositions and the half life of the two isomers.An explanation is offered for the fact that the final conversion X∞ of 1 and 2 at lower temperature is larger than that of 1 and 2 at higher temperature in terms of the comprehensive constant k' of the kinetic chain length.
    Studies on O-s-(2'-OR4'-Pyridyl)Propyl Phosphorothionates,Phosphonothionates and Phosphoroamidothionates
    Chen Ruyu, Liu Zhun, Cao Guifang, Fang Jianxin
    1987, 8(12):  1096-1101. 
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    Eighteen new O-3-(2'- or 4' -pyridyl)propyl phosphoronates (Ⅰ), phospho-roamidothionates (Ⅱ) and phosphonothionates (Ⅲ) were prepared by condensing 3-(2'-or 4-pyridyl) propanol with O, O-dialkylphosphorochloridothionates(1) O-alkylphosphoroamidochloridothionates (2) and O-alkyl (or aryl)phenylphos-phonochloridothionates(3), respectively, in presence of a base. The favourable reaction conditions and the purification methods of these compounds were found out. Their 1R and 1HNMR spectra data were given. The results of the primary biological tests showed that some of the compounds enhanced and some inhibited the growth of the coleptiles of wheat.
    Crystal and Molecular Structure of Meso and d l-2,3 -Diethoxy-2,3-Diphenylsuccinonitriles--The Influence of Capto-dative Effect upon the Conformation of the Molecules
    Liu Zhongli, Wang Panfen, Wu Longmin, Liu Youcheng, Meng Yimin, Wang Xin, Zhu Ying, Wang Qiguang
    1987, 8(12):  1102-1106. 
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    The crystal and molecular structure of meso- and dl-2,3-diethoxy-2,3-diphe-nylsuccinonitriles, 1a(meso)and 1a(dl), which are substituted ethane derivatives with capto-dative substituents, have been determined by X-ray crystallography. It is found that the central carbon-carbon bonds and chemical bonds attached to them are all obviously stretched. The deformation of the molecules is explained by steric, electronic and capto-dative subtituent effects through conformational analysis.
    Synthesis of the Components of San Jose Scale's Sex Pheromone 3,7-Dimethyl-2,7-Octadien-1-yl Propionate
    Chen Jiawei, Zhang Hesheng, Jiang Jilong, Xu Zhanghuang
    1987, 8(12):  1107-1109. 
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    The components of San Jose Scale's sex pheromone Z- and E-3,7-dimethyl-2,7-octadien-1-yl propionate have been synthesized in the ratio of 25:75 from ethyl aceto-acetate and ethyl acrylate in ten steps in an overall yield of 9 %.
    Research on Synthetic Method of 2,6-Disubstituted Benzo-Bisoxazoles
    Wang Mingzhen, Pan Jiaxing, Zhou Yimin, Gao Zhenheng
    1987, 8(12):  1110-1112. 
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    In this paper a modified method of preparation of 2,6-disubstituted benzo-[1, 2-d;4,5-d']-bisoxazoles is reported.2,5-Diamino-quinone-1,4 was reduced with stannous chloride in hydrochloric acid. The product, 2,5-diamino-hydroquinone-l, 4 hydrochloride was then condensed with benzoic acid and substituted benzoic acids respectively in polyphos-phoric acid. Thus, 2,6-diphenyl benzo-[1,2-d;4, 5-d']-bisoxazole and eleven of its substituted phenyl derivatives were prepared.
    The Phase Transfer Catalysis by PEG in Perkin Reaction
    Kang Ruhong, Zhang Yue, Huang Fengchen
    1987, 8(12):  1113-1117. 
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    Perkin reactions under phase transfer catalysis of poly(ethylene glycols)(PEG) were studied. It was shown that PIGgave a obvious catalylical effect on the reactions. PEG-600 of average molecular weight were more efficient than the others examined. The yields of Perkin reactions with PEG-600 were higher than that without it by 10%. Morever, the reaction time was shortened remarkably. Appropriate amount of PEGused in the reactions was ca. 1% (mole).
    ESR Imaging (Ⅰ)--The One Dimensional X B and Imaging of TEMPOL Aqueous Solutions
    Zheng Yingguang, Xu Yushu, Qiu Zuwen
    1987, 8(12):  1118-1120. 
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    One dimensional ESR imaging has been achieved using anti-Helmholtz gradient coil on Bruker ER 200D X-b and ESR spectrometer. Examples are presented using TEMPOL aqueous solution. Finally, a preliminary two-dimensinal imaging is also included.
    The Determination of Trace Amounts of Cadmium by Catalytic Kinetic Fluorometry
    Xu Jingou, Huang Xianzhi, Gu Qun, Fu Qinghui
    1987, 8(12):  1121-1123. 
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    A new method of catalytic kinetic fluorometry has been established for the determination of trace amounts of cadmium. It is based on the catalysis of both Cd(Ⅱ) and imidazolc on the reaction of complex formation between Co(Ⅲ) and α,β,γ,δ-tetrakis(4-sulphophcnyl) porphine [T(4-SP)P] in H3BO3-Na2B4O7buffer solution with pH8.5. Fixed time method is used in measuring the reaction rate. The concentration of the product, Co(Ⅲ)-T(4-SP)Pcomplex, is monitored by measuring the flourescence intensity of T(4-SP)Pwhich is decreased as the concentration of the product increases. The calibration graph is rectilinear over the concentration range of 0-16 ng Cd(Ⅱ)/ml. The limit of detection is 0.5 ng Cd(Ⅱ)/ml, the accuracy of determination,±6%. Eight replicate determinations of solutions containing 0.2μg Cd(Ⅱ) show a relative standard deviation of 4.3%.
    Synthesis and Properties of Silicone Supported Transition Metal Complex Catalysts (Ⅹ)--Catalytic Behavior of Poly-γ-(m-diphenylphosphinophenyl)pro-pylsiloxane Platinum Complex in Hydrogenation Reaction
    Lu Xueran, Xu Ping, Feng Minhua, Chen Yuanyin
    1987, 8(12):  1124-1126. 
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    A new polymer-bound complex catalyst, fumed silica supported poly-γ-(m-diphenylphosphinophenyl)propylsiloxane platinum complex, has been synthesized starting from γ-(m-chlorophenyl)propyltrimethoxysilane via phosphination with lithium diphenyl phosphide and then immobilized on silica followed by treating with potassium chloroplatinite. Nitrobenzene, 1-hexene, styrene and acrylnitrile were used as substrates to evaluate the catalytic behavior of the title catalyst in catalytic hydrogenation reaction. The structure of the catalyst was characterized by IR, XPSand elemental analysis.
    Molecular Motion of Star-Shaped Polystyrenes in Solution Studied by Carbon-13 NMR(Ⅰ)
    Wang Han, Hua Shiying, Li Ying, Qiu Zuwen, Shen Jiacong
    1987, 8(12):  1127-1130. 
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    The carbon-13 NMR spin lattice relaxation times,line widths and Nuclear Over-hauscr Enhancements were measured for solutions of regular star-shaped polystyrenes in o-dichlorobenzene and in CDCl3. The factors, molecular weight, concentration, solvent and molecular structure,which control magnetic relaxation, were examined. The experimental data were interpreted in terms of the log-X2distribution of correlation times
    Modification of Poly(Vinyl Chloride)(PVC) by Blending It with Chlorinated Polyethylene (CPE) (Ⅱ)
    Chang Eanghua, Zheng lun-wen, Song Moudao, Ding Peiyuan, Zhang Qihua, Ning Shunli
    1987, 8(12):  1131-1135. 
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    The effect of CPEchain structure on the modification of PVCblend has been studied by infrared spcciroscopy (IR), and differential scanning calorimetry (DSC). Dynamic mechanical spectra of the PVC/CPE blends indicate that they are partially compatable two phase systems. The morphology of the PVC/CPE blends were observed by transmission electron microscopy (TEM). High-impact strength of the PVC/CPE alloy is obtained when the rather regular network structure of CPEis formed.
    Influence of a Magnetic Field on the Closs-Linking of Epoxy Novolac
    Chen Yirui, Fan Zhengang, Fang Dongpu, Yao Kangde
    1987, 8(12):  1136-1140. 
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    This Paper discuss the effect of a uniform static magnetic field on cross-linking of an cpoxy Novolac cured with 2,4,6-tri (dimethylaminomethyl) phenol (DMP-30). The cross-linking reaction was canied out at 130-190℃. The change of ether bond linked network formed in structure was monitored by the determination of specific resistivity qualitatively. Results shewed that the magnetic field effect can promote the cross-linking reaction. It was verified by the FT-IR spectra analysis and observation under SEM. The improvement in cross-linked network led to an enhancement of resistivity on one to two orders of magnitude higher than of the control sample and increase in glass transition temperature.
    A Lewis Acid Catalyst Supported by Polymer--Polystyrene-AICI3/SnCI4Dibasic Metal Chloride Complex
    Fan Ruicheng, Jia Xinru, Wu Xianghong, Pei Weiwei, Jiang Shuojian
    1987, 8(12):  1141-1145. 
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    Polystyrene-divinylbenzene(4%) beads were combined with anhydrous aluminium chloride and stannic chloride (1:1) in chloroform to form a stable complex containing 7.73% of chlorine, in which the ratio of metal aluminium to metal tin is 2/1. It correspond to (0.278 mmol SnCl4+ 0.557mmol AlCl3)/1g complex beads. The complex beads (PS-Al/Sn) can be used to catalyze a lot of organic reactions, such as esierifications, acetalizations, ketal formations, ethe-rification and the Friedel-Crafts alkylations. The greater reactivity of the PS-Al/Sn compared to PS-A1Cl3(6) and PS-SnCl4(7) was confirmed in these reactions. It is important that the dibasic metal complex PS-Al/Sn as a fine catalyst can be reused at least 10 times in high yields.
    The Conformation of Molecular Segmer
    Zhang Xuesong, Shen Jiacong
    1987, 8(12):  1146-1149. 
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    There are approximately three conformation states of molecular segment, namely trans T, gauch G+, gauch G-. The conformation of segmer is determined by distribution of these states just like three component copolymer. We assign three kinds of distribution as following.By exact calculation the conformation for odd number of T-segment between two Gstates is different from that for even number, so we get six conformation of segmer. If we fix one end of segmer on same point, then these segmers walk to six nearly perpendicular direction in three dimension scale. In view of the above result, we propose some concept for amorphous structure of polymer.
    Determination of the Pore Structure of Porous Materials by Gel Permeation Ghromatography(GPC)--Determination Outside the Column
    Yan Juntan, Du Yingjun, Huang Mingde, Xu Rongnan
    1987, 8(12):  1150-1152. 
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    A new method for determining the pore structure of porous mate-rials outside the column by GPC (OGPC) has been proposed. This method can determine the pore structure of certain porous materials with a suitable solvent so that the simple equation governing elution in GPC can be applied.An equation for this method was deduced. The results of mcsurement on a sample of silica packing material were found to be satisfactory. An explanation for discrepancies in measurements on macroporous ST-DVB copolymers(which really contain also micropores) was proposed.
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