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    24 June 1989, Volume 10 Issue 6
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    Articles
    Investigation of Complex Reaction Between Extractant Molecules by Dielectric Measurements
    Peng Qixiu, Shi Xiukun, Wu Ming, Gao Hongcheng
    1989, 10(6):  561-565. 
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    The molecular dipole moment, as a very useful parameter for structural studies, has been applied to study the intermolecular interaction, such as association reaction, etc., between two extractants or extractant and extraction complex.The molar polarizabilities Pand dipole moments μ of some important extractants containing phosphorus TBP, TOPO, TBPO, P204, DBP, HDiAP, DiAEPin benzene were determined by use of dielectric measurements. These results are summarized in Table 1.Molecular-interaction between acidic and neutral extractants containing phosphorus has been studied by the same method. These formation constants Kc, molar polarizabilities Pand dipole moments μ of complexes are shown in Table 2.Dielectric property of mixed solution can be applied to the study of synergistic extraction systems.
    Synthesis and Magnetism of Binuclear Copper(Ⅱ) Complexes with N,N'-i,2-Propanedi- salicylamidatocuprate (Ⅱ)
    Liao Daizheng, Zhao Qianhua, Wang Genglin
    1989, 10(6):  566-570. 
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    New metal complexes of [Cu(sampn)CuL] type were synthesized, where sampn4- denotes N,N'-1,2-propanedisalicylamidate anion and Ldenotes 2,2'-bipyridyl(bpy) or 1,10-phenanthroline(phen). Based on IR, elemental analyses and electronic spectra, the complexes are proposed to have phenoxy-bridged structure and to consist of the Cu(Ⅱ) in distorted planar environment. The complexes have been characterized with variable-temperature magnetic susceptibility (77～300K)and the observed data were fit to those from a modified Bleaney-Bowers equation by means of least-squares, resulting in a larger θ. This suggests that two binuclear units have a considerable intermolecular interaction.
    The Sensitization of Tb3+ Luminescence by Ce3+ in Lanthanum Silicophosphates
    Huang Zhupo, Ma Guoling
    1989, 10(6):  571-574. 
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    We studied the emission and excitation spectra of Tb3+-activated as and Ce3+ and Tb3+-coactivated 2O3·0.01 SiO2·0.95 P2O5. Though the comparison between emission and excitation spectra, we have found that luminescence of Tb3+ is greatly sensitized and enhanced in the presence of Ce3+ .The effect of temperature on the luminescence of Tb3+- activated as well as Ce3+ and Tb3+ -coactivated phosphorus was studied.The energy transfer efficiency from Ce3+ to Tb3+ was calculated to be more than 95%. The mechanism of energy transfer from Ce3+ to Tb3+ has been shown to be a resonance process.The phosphorus shows different concentration quenching conditions under various types of excitation. The higher the excitation energy, the smaller the concentration at which the quenching starts to occur. The optimum concentration for Tb3+ emission under different excitations was determined.
    Simultaneous Determination of Phenol and Resorcinol in Pharmaceutical Preparations by Kalman Filtering-Spectrophotometry
    Li Zhiliang, Liu Yiming, Yu Ruqin
    1989, 10(6):  575-580. 
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    UVspectrophotometry based on Kalman filtering (KF) was applied to the simultaneous determination of phenol and resorcinol in synthetic mixtures and pharmaceutical preparations without preliminary separation. The average recoveries for phenol and resorcinol in their compound preparations are 100.86% and 98.76%, with standard deviations of 1.58% and 1.66%, respectively.
    Studies on the Synthesis of Bromodimethylaminoaniline-fluorone and Its Colour Reaction with Iron
    Yang Bailing, Yu Ximao, Yu Xiaomei
    1989, 10(6):  581-585. 
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    Ahighly sensitive colour reagent bromodimethylaminoaniline-fluorone (BDMAF) was synthesized and identified. The colour reaction of BDMAFwith iron in the presence of auxiliary complexing ligands and surfactants was studied systematically. The blue quaternary complex of Fe-acetylacetone-BDMAF-CTMABexhibits absorption maximum at 608 nm with an apparent molar absorptivity of 1 .6 × 105 L.mol-1 .cm-1 in the medium of NH3-NH4C1 buffer of pH 9.5～10.5. Its apparent stability constant is 6.8×1012. Beer's law is obeyed for iron of 0～5.5 mg/25 L. The composition of this complex was found to be Fe( Ⅲ):BDMAF = 1:2. The method has a high selectivity in the presence of 'EGTA, it has been applied to the determination of trace amounts of Fe3+ in zinc alloys without separation. The variation coefficients are 3.2%～3.9% for the four standard samples of zinc alloys measured (7 times).
    Simultaneous Determination of Samarium and Gadolinium in Their Concentrated Material in the Process of Rare Earth Production
    Wang Lisha, Cai Ruxiu, Zeng Yun'e
    1989, 10(6):  586-590. 
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    This paper deals preliminarily with the substitution reaction mechanism of RE(DBC)3(DBC = 2-(2-arsenophenylazo)-7-(2, 6-dibromo-4-chlo-rophenylazo)-1,8-dihydroxynaphthalene-3,6-disulfonic acid) with CyDTAbased on the experimental facts and theory deduction. Akinetic reaction system for simultaneous determination of Sm and Gd was established by choosing the best substituent and complexing agent from several aminocarboxylic acids and polyhalidarsenazoes. Under the suitable conditions Sm and Gd in their concentrated material were determined simultaneously in this kinetic reaction system. The result agrees satisfactorily with that obtained by JCP-AES. The synthetic samples of Sm and Gd mixture with a content ratio in the range of 1:2～4: 1(Sm:Gd) were determined by this method. The error of it is about 10%. It is predictable that the method would be used for a control of procedure in the rare earth production.
    Studies on the Polarographic Adsorptive Wave of Isonuclear Complex of Rare Earth-Zinc- Alizarin Complexon
    Li Nanqiang, Wu Danan
    1989, 10(6):  591-595. 
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    In the 0.2mol/Lacetate buffer solution, at pH 4.8, a sensitive adsorptive wave of RE( Ⅲ)-Zn( Ⅱ )-ALCisonuclear complex was obtained by means of single-sweep polarograph with the exception of scandium. The limit of detection is 2.0×10-8 mol/Lfor light rare earth ions. The composition of the isonuclear complex was determined as RE( Ⅲ ):Zn( Ⅱ ):ALC = 1: 1 :2 by using the polarographic continuous variation method and the analysis of the isonuclear complex precipitate. The electrode processes of the adsorptive wave may be represented as follows:(这里有图片1989067-591-1.gif)where L' is the anthrahydroquinone anion of ALC.
    Analytical Behavior of Mercury Film Carbon Fiber Electrodes in Differential Pulse Stripping Voltammetry
    Peng Tuzhi, LU Rongshan
    1989, 10(6):  596-600. 
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    This paper reports the behavior of trace metals at mercury film carbon fiber electrodes in differential pulse stripping voltammetry. In comparison with glassy carbon electrodes and hanging mercury drop electrodes, carbon fiber electrodes show many advantages in quiescent solution, dilute solution, organic solution and a double-electrode system. This paper discusses the preparation and pretreatment of carbon fiber electrodes and the measurement conditions.
    Studies on Cp2ZrCl2-i-BuMgBr Reagent System—Reductive Dipolymerization of defines and Enynes, and Intramolecular Cyclization of Dienes
    Wu Shaozu, Zhang Yulan, Isagawa Kakuzo, Otsuji Yoshio
    1989, 10(6):  601-604. 
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    Treatment of Cp2ZrCl2 with 2 equivalent of i-Br.MgBr Grignard reagent in THFat room temperature produces organo-zirconium species that react with alkenes, alkynes or diencs, ending up with reductive dimers or intramolecular cyclization products.
    Synthesis of Amino Acid 5-Fluorouracil Esters Derivatives and Study on Their Antitumor Activity
    Zhao Rulin, Fan Changlie, Zhuo Renxi
    1989, 10(6):  605-608. 
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    Eighteen amino acid 5-fluoroiu-acil-propyl(butyl) ester hydrochlorides were synthesized by the reaction of N-protected salts of amino acids with 1-(w-bromopropyl)-5-fluorouracil and 1-(w-bromobutyl)-5-fluorouracil in DMF. The structures of these new compounds were characterized by 1H NMR, IRand UVspectra, as well as elemental analysis, Tyrosine and phenylalanine 5-fluorouracil-propyl ester hydrochlorides show an inhibition ratio of 88.1% and 86.7% respectively against Ehrlich Ascites Carcinoma in mice.
    Determination of Characteristic Composition 10-Hydroxy-2-Decenoic Acid in Royal Jelly by High Performance Liquid Chromatography
    Zhang Xie, Fu Chunyan, Yang Renfei
    1989, 10(6):  609-613. 
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    Amethod for the quantitative determination of 10-hydroxy-2-decenoic acid (10-HDA) in royal jelly(RJ) and RJpreparation was established by high performance liquid chromatography (HPLC).The lo-HDAextracted with dichlo-romethane from royal jelly or royal jelly preparation was determined by HPLC. The system was recommended on a YWG-C18 column (φ4.6×250 mm) using 35% ethanol in water (pH = 2.5) as the mobile phase; detection of ultraviolet absorption was performed at 212 nm, and at the range of 0.16 AUFS; internal standard, adipic acid.This method was successfully applied to the determination of 10-HDAcontents in raw royal jelly, ginseng royal jelly and ginseng pilose antler royal jelly. It is simpler, more rapid than and superior to gas chroma-tographic and thin-layer chromatographic methods.
    Selective Synthesis of N,N-dimethylaniline(DMA) over Zeolites
    Wu Kerui, Fu Jun, Hou Zhenshan, Yao Xiuzhi
    1989, 10(6):  614-618. 
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    The selective synthesis of N,N-dimethylaniline (DMA) from aniline and methanol was studied over modified ZSM-5 zeolite. At 300℃, under an ordinary pressure,LHSV= 1.0h-1,and aniline:methanol = 1:3,the modified ZSM-5 catalyst was found to show 88.5% selectivity for DMAat the conversion level of 97.8% for aniline, indicating obvious applied prospect.
    Alumination of ZK-4, Sodalite and NaA Zeolite
    Zhao Dating, Zhang Ping, Pang Wenqin
    1989, 10(6):  619-622. 
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    Alumination of ZK-4, sodalite and NaAzeolites was carried out by gas-solid replacement reaction at a high temperature. Chemical analysis, effluent gas analysis, XRD, IR, SEMand 29Si magic angle spinning NMRshowed that the Al-O-Al linkage is likely present in the framework of aluminated-ZK-4, aluminated-sodalite and aluminated-NaAzeolites after the three kinds of zeolites were aluminated at a elevated temperature.
    Studies on Synthesis, Phase Transfer Catalysis and Catalytic Mechanism of Polystyrene-Supported Polyethylene Glycol Benzyl Ether
    Liang Xun, Qi Hongyan
    1989, 10(6):  623-628. 
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    Polystyrene-supported polyethylene glycol was synthesized using a imporved method. The phase-transfer catalysis was studied in the reaction of n-C8H17Br with solid Nal. The reaction rate was a first-order with respect to the concentration of n-C8H17Br. The observed reaction rate constant kobs increased as the degree of cross-linking and particle size of catalyst decreased. Macroporous catalysts showed a higher activity than that of microporous catalysts. Trace amount of water also showed some influence on kobs. kobs of PEGwas increased after it was immobilized. The solid-solid contact mechanism of S-S-Lsystem was confirmed by our experiment.
    Studies on Multipurpose VLE Determinating Apparatus
    Zhou Xingfeng, Ni Liang, Han Shijun
    1989, 10(6):  629-633. 
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    This Paper presents a newly designed multipurpose VLEdeterminatingapparatus—CS- Ⅱ VLEdeterminating apparatus and discusses the ideas of theapparatus design. With the features and functions of both VLEstill and ebulliome-ter, it has a pump-like stirrer so that it can be used appropriately to quasi-static method; it has a new structure of sampling vessels and valves, which makes it applicable to both miscible and partially miscible solution systems and appropriate to the system with high boiling temperature difference of components. The detail results of the experimental verification are given in this paper.
    Thermotropic Liquid Crystalline Sequential Block Copolyesters
    Li Zifa, Zhang Ziyong, Zhou Qifeng
    1989, 10(6):  634-637. 
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    Aseries of sequential block copol'ymers was synthesized by polycon-densation of 1,10-decanediol, poly(oxytetramethylene)glycol (MW=1050) and the mesogenic monomer 2-methyl-p-phenylene di(4-chloroformyl)benzoate. These polymers were found to be liquid crystalline when the feed ratio of poly(oxytetramethylene)glycol to 1,10-decanediol was less than 70 to 30. The mesomorphic behavior of these polymers was characterized by a polarizing microscope, a DSCinstrument and a X-ray diffractometer.
    Studies on Synthesis and Application of Porous Carrier for Solid Phase Radioimmunoassay
    You Yingcai, Liang Xun, Teng Xinlian, Guo Xianquan, Hou Bingzhang, Yin Boyuan
    1989, 10(6):  638-641. 
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    Porous microspheres with diameter ranging from 250 to 400 mesh and pore sizes from 1524 to 4304Å were synthesized by suspension polymerization of MMAand DVBwith 26-50% paraffin liquid or 30-50% 200# petrol by weight as porogenic agents. The microspheres extracted with petroleum ether were hydrolyzed (50% NaOH, 140-150℃; 1-5 h). The microspheres with spacer were prepared by reacting carboxylated microspheres with 1,6-hexamethylene diamine. The T4 -anti-body was covalently coupled to the microspheres with spacer by a two-step glutaraldehyde method. The reactivity of the microsphere-anti-body conjugates was characterized by reacting the microsphere-anti-body conjugates with 125Ilabeled thyroxine, the binding percentage is 94%.The results of our experiments showed that the porous microspheres is a ideal carrier for solid phase radioimmunoassay of thyroxine.
    Molecular Orbital Theory on Chain Conjugated Polymers (Ⅳ)— General Condition for Factorizing the Eigenequation of Repeating Unit Systems and Its Boundary States
    Li Jiabo, Yang Zhongzhi, Ye Yuanjie, Tang Aoqing
    1989, 10(6):  642-643. 
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    The relationship between the local symmetry of chain conjugated polymers and the angle of the complex bottom vector D(λ) is given. Based on it, the general condition for the factorizing the eigenequation of chain conjugated polymers is obtained. The analytical form of boundary states is given. It suggests a method to investigate the effects of the size and boundary of polymers.
    The Formation of New Porphyrin Species(NPS) from Hematoporphyrin Derivatives (HPD) in Sodium Saline Solution by Standing away from the Light
    Qiu Yuluia, Zhang Weide, Yan Xueming
    1989, 10(6):  644-646. 
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    After HPDin sodium saline solution standing away from the light, NPSis formed. It shows an absorption/excitation peak at 403 nm, an emission peak at 580 nm. Its formation is strongly influenced by many factors, in particular, irradiation, temperature, pH, concentration and gases diluted in thesolution. NPSwas tentatively identified as a complexing intermediate ------"thesitting-at top complex" formed by combining HPDwith sodium ion in the solvent. The formation of NPSprobably brings about unfavourable influence upon the photosensitive capacity of HPDin cancer tissues.
    Study on McReynolds Constants of Eight Crown Ether Stationary Phases
    Shi Jian, Lu Guoyuan, Guo Wei, Wang Defen, Hu Hongwen
    1989, 10(6):  647-649. 
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    In this paper; the chromatographic characterization of eight crown ether stationary phases is relatively and comprehensively discussed through the determination of their McReynolds constants and in comparison with typical stationary phases. The reason for having different McReynolds constants for the crown ethers is attributed to the differences of their structures. Special uses for some crown ethers are introduced. The accuracies of the constants were tested and verified.
    Stereoselective Synthesis of3,5-Cyclo-Pregnane-6- Methoxyl-20-S-22-Aldehyde
    Liu Xing ping, Li Yulin, Liang Xiaolian
    1989, 10(6):  650-652. 
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    The stereoselective synthesis of 3,5-cyclo-pregnane-6-methoxyl-20-S-22-aldehyde(7),which is the key intermediate of the synthesis of brassinolide(1) and its analogous, was carried out with diosgenin as starting material. In this reaction the e,e is 86.2%.
    Study on the Synthesis of Some New Biflavonoids (Ⅴ) —Total Synthesis of 0-Hexamethyl Brackenin
    Li Yulin, Zhu Jieping, Zhang Fangjie, Wang Qian
    1989, 10(6):  653-654. 
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    O-Hexamethyl brackenin ( Ib) was first successfully synthesized by using resorcinol as starting material. According to the same synthetic route, the other two dimeric dihydrochalcones ( Ic, Id) were also synthesized.
    Synthesis of 1,3,2-Diazaphospholidines
    Chen Ruyu, Liu Zhun, Li Chenxi
    1989, 10(6):  655-657. 
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    The reactions of N, N' -bis (substituted benzenesulfonyl) ethylenedi-amine with phosphites and hexaalkyl phosphorous amides were studied. It was found that N,N'-bis(substituted benzenesulfonyl)ethylenediamine could not react with phosphites, but could do with phosphorous amides to form 1,3,2-diazaphos-pholidines. NMRand MSspectra of 1,3,2-diazaphospholidines were discussed.
    Crown Ether Derivatives of EDTA (Ⅴ)—Synthesis of EDTA-Diaminodibenzocrown Ether Polyconden- sate and Preliminary Study on Their Adsorption Behavior for Some Metal Ions
    Qin Shengying, Liu Zhongqun, Chen Shaojin, Jin Chengchang
    1989, 10(6):  658-660. 
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    EDTAdianhydridc reacted with 4,4' -diaminodibenzocrown ethers or 4,4'-diaminobiphenyl to give polyamido acids 3a-d, bearing pendant carboxymethyl groups on the chain. 3a-d were heated under vacuum to form polyimides 4a-d. The adsorption behavior of the polymers for U(Ⅳ)> U(Ⅵ), Au(Ⅲ) and K( Ⅰ ), etc. was examined. The preliminary experiment shows that the polyamido acids are superior to the polyimides in adsorbability for some metal ions and the cis-polyamido acid 3d, is the most excellent one among the 8 polymers. 3a has the capacity of 97.5 mg U(Ⅵ)/g, 976 mg Au(Ⅲ)/g and 10.6 mg K(Ⅰ)/g, respectively.
    Composition of HZSM-5 Zeolites and Its Effect on the Selectivity of Toluene Ethylation
    Liu Shangyuan, Liu Shuangxi, Sun Mingyong
    1989, 10(6):  661-663. 
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    The shape selectivity for the alkylation of toluene with ethanol by varying Si/Al ratios of HZSM-5 and DAI HZSM-5 zeolites was studied. The results show that p-ethyltoluene selectivity increases with the zeolite Si/Al ratio increase. By treating HZSM-5 zeolite with SiCl4 vapor, the aluminium atoms were removed, indicating that the surface is deficient in aluminium obviously. At a high temperature and within short time, especially, HZSM-5 zeolites treated by SiCl4 showed obviously a higher p-selectivity, but the activity had no clear change.
    Measurement of Primary and Secondary Kinetic Deuterium Isotope Effects by Natural Abundance2H NMR(Ⅲ)—Application to the Hydrolysis of Some Grignard Reagents
    Zhang Benli, Li Guigen, Gao Zhenheng, Wu Jiazhen
    1989, 10(6):  664-666. 
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    We established a method of using natural-abundance 2HNMRfor the study of kinetic deuterium isotope effects (KDIE) which is based on the determination of site-specific isotope ratios of hydrogen in the molecules involved in the reaction. It was applied to the KDIEstudy of the hydrolysis of two Grignard reagents, benzylmagnesium chloride and phenylmagnesium bromide for which kH/kD= 1.52( ±0.03) and 1.50(±0.04), respectively.
    The Effect of Magnetic Field on the Emulsion Polymerization of Vinyl Acetate
    Su Zhixing, Yao Fanglian, Zhang Ping
    1989, 10(6):  667-669. 
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    This paper reports the effects of a magnetic field on the emulsion polymerization of vinyl acetate initiated by oil-soluble photo-sensitized initiator, benzoin. It was found that the polymerization rate and molecular weight of the polymer increase with the increase of magnetic field intensity in a lower magnetic field, and decrease fastly with increasing magnetic field intensity in a higher magnetic field.
    Study on Radiation-Induced Crosslinking of Polyethylene Swollen in Some Organic Molecules
    Ha Hongfei
    1989, 10(6):  670-672. 
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    Radiation-induced crosslinking and the changes of unsaturation of polyethylene swollen in n-hexadecene-1 and n-hcxadecane, respectively, at room temperature were investigated. There were marked decreasing of crosslinking and obvious changes of unsaturation for the samples swollen in both of the organic molecules under irradiation without oxygen. The results show that Ytype crosslinking of irradiated polyethylene is the main crosslinking type.
    Aqueous Polymerization of Acrylamide Initiated by K2S2O8-Urea Redox
    Liu QingPu, Ha Runhua, Liu Hongrong, Hu Jinsheng
    1989, 10(6):  673-675. 
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    The kinetics of aqueous polymerization of acrylamide initiated by potassium pcrsulfate and urea was investigated. The results arc sumarizod in the empirical expression, Rp<∝[AM]1.5CK2S2O8]0.45[CO(NH2)2]0 in the range of CK2S2O8]= (1.036～7.542).10-5m0l/LandCCO(NH2)2= (0.479～47.930)-10-4 mol/L.The overall activation energy of polymerization equals 51.27 kJ/mol which confirms that this initiation is a redox reaction. The effect of urea on molecular weight of the polymers is discussed.
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