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Table of Content

    24 March 1990, Volume 11 Issue 3
    Articles
    Syntheses and Properties of Adducts between Heteropoly Tungstic and Molybdic Acids and Their Salts and N,N-Dimethyl Formamide
    Gu Yidong, Ding Jianping
    1990, 11(3):  221-225. 
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    The adducts between heteropoly tungstic and molybdic acids and their salts and N, N-dimethyl formamide (DMF) were synthesized and characterized by IR, Raman, UV-VS, 1Hand 13C NMRspectrometry, TG-DTAthermal analysis and X-ray diffraction analysis. The IRand NMRspectra showed that the coordinating atom of DMFwas oxygen of C = Obond, and the shift of C = Ovibration frequency might be considered as the criterion of M-Obond strength. The organic ligands do not coordinate with heteropoly anions, but with protons in heteropoly acids by hydrogen-bond, or metal cations in heteropoly tungstates and molybdates by coordination bond. The X-ray diffraction analysis showed that the DMFadduct of CaPWis monoclinic, and its space group is C52k-P21/n, with unit cell parameters; a = 12. 927(7) Å, 6=33.850(9) Å, c=17. 903(13) Å, B=106.78(4), V=7500. 37 Å3.The figure of merit is F=M9(0. 016, 38).
    Structural Studies on Rare Earths Carboxylates( Ⅱ ) —Synthesis,Characterization and Structure Determination of Nitrate Di(2-Ethylhexanoate) Di(Ethyl Alcohol) Neodymium
    Li Junran, Huang Chunhui, Li Biaoguo, Xu Guangxian
    1990, 11(3):  226-230. 
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    The synthesis, the crystal and molecular structure of neodymium complex NdA2NO3(C2H5OH)2(A= 2-ethyl hexanoate group) are presented in this report. The crystal and molecular structures were determined by single crystal X-ray diffraction techniques with a four circle diffrac-tometer to give a final Rvalue of 0. 0997. The crystal is triclinic with a space group P1. The unit cell parameters are:a = 9. 448(4)Å, b= 12. 146(4)Å, c= 12. 974(5)Å, a=71. 56(3)°, β = 98.45(3)°, γ=98.62(3)°, V=1388.6(9) Å3, Z = 2, dcalc=1. 397 g/cm3. Each two neodymium atoms in crystal are connected with two bridging carboxyl groups to form a chain polymeric molecule. The middle point of the linking line of two neodymium atoms is on the axis a. In addition, every neodymium is coordinated by 4 oxygen atoms. Two of them are from a bidentate nitrate, and the others from two ethyl alcohol molecules. The coordination number of neodymium is 8 and the coordination polyhedron of neodymium takes an arrangement of a distorted delta dodecahedron.
    The Determination of Standard Molar Enthalpies of Formation for Complexes of Rare Earth Isothiocyanates with Dimethylsulfoxide
    Yin Jingzhi, Jiang Bengao, Sun Tongshan, Suo Zhanghuai
    1990, 11(3):  231-235. 
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    The preparation of seven solid complexes of rare earth isothiocyanates with dimethylsulfox-ide(DMSO) was reported. Their chemical formulae were proved to be RE(NCS)3·5DMSOwhere REis La, Ce, Pr, Nd, Sm, Eu, Gd. By means of the thermochemical method, the standard molar enthalpies of formation of these complexes were determined and their lattice energies were calculated.
    Study on Trace Lead Ion-Exchange on Nation-Modified Electrode and Its Determination
    Jin Litong, Liu Bin, Fang Yuzhi
    1990, 11(3):  236-239. 
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    Using the properties of Nation membrane making ion-exchagne with trace Pb( Ⅲ) in solution, this paper describes the method of Nafion modified electrodes concentrated and determination of Pb( Ⅱ), and discusses its reaction mechanism. There is a linear rlationship between the concentration and peak height in the range of 13-133 ng/mLfor Pb( Ⅱ ), the variation coefficient for the method is 3. 5%, the detection limit of Pb( Ⅱ) is 6 ng/mL.
    Spectrophotometric Determination of Compositions and Stability Constants of Coordination Compounds in Mononuclear and Polynuclear Coexistent Systems
    Zou Shifu, Cao Wei, Wen Shiqi
    1990, 11(3):  240-244. 
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    Isobestic point spectrophotometric method is proposed to determine the compositions and stability constants of complexes in a coexistent system of mononuclear and polynuclear complexes. This method has been used in a indium-xylenol orange system, the compositions of the two complexes obtained are 1:1 (In:XO,λmax=510 nm) and 2:1(λmax=560 nm), and the stability constants are K1 = 8. 83×108 and K2=1. 44×107, respectively.
    Kalman Filter Fluoremetry and Its Application to Simultaneous Determination of Mixture of Fluorescent Dye
    Li Zhiliang, Shi Leming, Li Menglong, Yu Ruqin
    1990, 11(3):  245-249. 
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    Anew method, Kalman filter fluoremetry, has been developed based on the characteristics and multicomponent Analysis model of conventional and synchronous fluorescence spectrometry. Several filtering procedures are examined and compared with each other. The tendency of state estimation, the reduction of error covariance and the irrelation of innovation sequence obtained from filtering process are investigated to be used as criteria to judge the assay reliability. The proposed method has been applied to determination of mixtures of the fluorescent dyes fluorescein, rhodamine Band rho-damine 6Gwith good results and with no separation.
    Application of Simplex-Deviation-Pattern Recognition to Studies of Adsorptive Polarographic Wave
    Zhang Zhengqi, Yu Ruqin
    1990, 11(3):  250-254. 
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    In this paper the simplex-deviation-pattern recognition is proposed and applied to the studies of adsorptive polarographic wave. With simplex-deviation-pattern recognition it is estimated that the adsorption of 2-QADNm and 2,7-TADNobeys Frumkin isotherm. The values of adsorption coefficient, interaction coefficient between adsorbant molecules and adsorption free energy were determined.
    Studies on Synthesis and Crystal Structure of Binuclear Complexes PdW(μ-Ph2Ppy)2(μ-CO)(CO)2Cl2 · 0. 7CH2Cl2
    Zhang Zhengzhi, Wang Xukun, Shen Yujun, Yao Xinkan, Wang Honggen
    1990, 11(3):  255-259. 
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    0CF.((, Anew complex containing Pd-Wbond, PdW(μ-Ph2Ppy)2(μ-CO)(CO)2Cl2 has been prepared and its crystal and molecular structure determined by X-ray diffraction. The molecule crystallized in the monoclinic space group P21/c with a=14. 616(3) Å, b=15. 289(1) Å, c=17. 676 (1) Å, β=97. 29(1)° and Z=4. the final R=0. 081. The palladium atom is d9 five-coordinated and the tungsten atom is d5 seven-coordinated. Both metal atoms possess the formal oxidation state +1. The molecule is chiral and belongs to the C1 point group.
    Studies on Synthesis and Their Photo-Properties of 2-(Substituted Styryl)-5-Substituted Benzoxazole
    Zhou Yimin, Zhao Xumiao
    1990, 11(3):  260-265. 
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    Twenty-two of the 2-(substituted styryl)-5-substituted benzoxazole compounds were synthesized by condensation of the corresponding2-methyl benzoxazole or 5-t-Bu-2-methylbenzoxazole with benzaldehyde, substituted benzaldehyde in the medium of KOH/DMFrespectively. Their m. p., vmax of UVspectra and fluorescence emission spectra, fluorescence quantum yields, as well as Stokes shifts of the compounds were examined. The solvent effect of compounds 1 and 15 was also discussed.
    Study on Bis Crown Ethers (Ⅶ)—The Syntheses of the Schiff Base Type and Secondary Amine Type Bis (Benzo-18-Crown-6)
    Wang Defen, Wang Dengjin, Hu Hongwen
    1990, 11(3):  266-270. 
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    Six new Schiff base type mono- and bis- crown ethers were prepared by condensing 4’-amino benzo-18-crown-6 with m-nitrobenzaldehyde, p-nitrobenzaldehyde, isophthalic aldehyde, substituted isophthalic aldehydes and terephthalic aldehyde respectively.Schiff base type bis- crown ethers were also prepared by the reaction of 4’ - formyl benzo-18-crown-6 with 4’-amino benzo-15-crown-5 and 4’-amino benzo-18-crown-6. Secondary amine type bis crown ethers were obtained by the reduction of the Schiff bases with sodium borohydride.
    An Electrochemical Study on Binuclear Big Bird Complexes of Ni( Ⅱ ) and Cu( Ⅱ )
    Luo Qinhui, Yang Sheng, Shen Mengctutng, Peng Qingyun
    1990, 11(3):  271-275. 
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    We studied by cyclic voltammetry the oxidation-reduction process of binuclear Big Bird complexes of Ni( Ⅱ ) and Cu( Ⅱ ). Big Bird ligand was synthesized by condensation of tert-buty 1-2,6-diformyl-phenol with 4-n- hexyl- thiourea. The interaction between two central atoms in binuclear complexes and their rate constants of electrode reaction were also investigated. Activation of COby Ni( Ⅱ ) complex was verified by IRand cyclic voltammetry.
    The Effect of Rare-Earth on Oxidization Catalyzed by Heteropoly Molybdovanadophosphoric Acid
    Wu Tonghao, Leng Yuchun, Yang Hongmao, Wang Guojia, Jiang Yuzi, Zhen Kaiji
    1990, 11(3):  276-279. 
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    The effect of the substitution extent of lanthanum and other rare-earth elements on oxidation reations of oxygen-containing organic compounds over heteropoly acid catalysts and the reactivity to correlate with structure of the catalysts are discussed. The addition of lanthanum does not change the activity of oxidative dehydrogenation, but lowers that of oxygen-addition reation apparently.
    Synthesis and Crystal Structure of Mixed Valence Pentadecavanadate V15O36Cl](NH4)3Na7·30H2O
    Shao Meicheng, Leng Jing, Pan Zuohua, Zeng Huadong, Tang Youqi
    1990, 11(3):  280-285. 
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    Using VOSO4 or VOCl2 as the starting materials, the title complex was prepared with additive agents NH2OH.HC1, NH2CH2COOHin the liquor with the final pHrange of 8-9 controlled by NaOH.The title complex crystallizes in space group D33h-P62m with unit cell constants a= 13. 111 (7)Å, c=11. 130(4)Å and Z=1 for chemical formula (V15O36Cl)(NH4)3Na7-30H2O. Those vanadium coordinates were derived by Patterson-minimum function method first and then the position parameters for the other non-hydrogen atoms were obtained by the Fourier difference techniques. Using 1084 independent reflections, the block-diagonal least-squares refinement for structural parameters gave final discrepency factor Rand Rw being<0.0353 and 0. 0344 respectively. X-ray structure analysis shows that in each unit cell two special positions with 3 symmetry are occupied by two (Na2(H2O)9)2+ groups and one 6m2 position is occupied by a chlorion-contained pentadecavanadate anion (V15O36Cl)10- in which there are 15 terminal-oxygen Oa, 3 bridged-oxygen Ob, 18 triple-linked Oc and three kinds of 15 Vanadium atoms. Carefully considering all the information of chemical bond parameters, hydrogen linking as well as the calculation results of bond-valence sum for all Vand Oatoms, we recognize that three V (3) atoms are in V (Ⅳ ) valence state and the rest 12 atoms of V (Ⅰ), V(Ⅱ) in IV-Vmixed valence state. The average occupation ratio of V( Ⅴ ) for V(Ⅰ) and V(Ⅱ) is - 0. 25 which implies the pentadecavanadate group belongs to a special kind of poly-vanadate group in which the V(Ⅳ) plays the main part in holding the back-bone of the cluster and tolerates some extent V( Ⅴ) residing in.
    Synthesis of Tetramethine-Styryl Cyanine Dyes and Their Lasering Properties
    Yang Jinlong, Zhu Zhenghua, Yao Zuguang
    1990, 11(3):  286-289. 
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    Aseries of tetramethine-styryl cyanine dyes are synthesised. Lasing properties of these dyes, including tuning range, center laser wavelength, conversion efficiency and stability, are examined with the pump source of the frequency-doubled mode-locked Nd : YAGlaser(532 nm). The relationship between molecular structures of dyes and their lasing properties was studied.
    Studies on Effects of Radiation-Induced Crosslinks in Polyethylene in Molten State by High-Resolution Solution13C NMR (Ⅱ)
    Zhu Qingten, Fumitaka Horri
    1990, 11(3):  290-294. 
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    Crosslinking structure formed during irradiation of polyethylene with the doses just lower than the gel dose,and the effects for this formation were investigated by 13C NMR Spectra. It is shown that formation of both "H" and "Y" type not only have a connection with irradiated doses, but also a few of other structures containing in the original PE. Nevertheless, are not related to the molecular weight for the PEsamples. The reaction mechanism and the principal factors influencing radiation-induced links arc also discussed for PEin the molten state.
    The Supposing and Proving of Hydroquinone Snake-Cage Redox Resin Structure
    Chen Xingqi, Liu Jianhua, Zuo Yumin, Zhang Shuling
    1990, 11(3):  295-299. 
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    In this paper, the snake-cage redox structure pattern of the resin is supposed in accordance with the theory of template polymerization and the experimental results on the redox properties of the resin, 717 cross-linking matrix resin(a Chinese commercial product) is considered to be"a cage", the linear hydroquinone-formaldehyde (in equal moles) polymer occluded within the matrix resin should be considered as "a snake",which has a redox function. The resin above is simply called HSR.The main experimental evidences of this structural pattern; (1) The snake-cage structure photographs of HSRhave been shown by electron microscope; (2) It has been proved by analysing the IRspectra of the extraction solution for HSR-tetrahydrofuran that hydroquinone-formaldehyde polymer in HSRis linear; (3) It was shown by using the spectra of HSRstanding in the oxidation or reduction state that there is an oxidation or reduction group in HSR,and the mutual change between the two kinds of groups can be carried out; (4) The experimental quantitative value of Nelement of HSRis consistent with that calculated according to our structural pattern.
    Synthesis and Characterization of VPI-5 and MCM-9 Molecular Sieves with Large Pores
    Qiu Shilun, Yao Shangqing, Pang Wenqin
    1990, 11(3):  300-301. 
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    Aluminophosphate-based molecular sieves of VPI-5 and MCM-9 were synthesized by hy-drothermal crystallization by using n- dipropylamine as a structure directing agent. The molecular sievies with large pores contain rings of 18 T-atoms. The synthesis conditions and crystallization were investigated.The structures and properties of the molecular sieves were studied by means of XRD, IRand TG-DTAtechniques. The results show that the VPI-5 is of a pure phase,whereas the MCM-9 is a mixture of VPI-5 and A1PO4-11.
    Studies on the Synthesis and Structure of Compound [H(napyo)2]ClO4
    Gan Xinmin, Wang Xin, Li Songlin, Tang Ning, Tan Minyu
    1990, 11(3):  302-304. 
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    The single crystal of compound [H(napyo)2]ClO4(napyo is 1,8-naphthyridine-N-oxide) was prepared in methanol medium. The crystal is a monoclinic system with space group P21/c. The unit cell parameters are: a=15. 602(2)Å, b=13.027(1)Å. c=8. 231(2) Å ,β=96. 47(1)°, Z=4. The proton in the compound is bonded to two oxygen atoms of two napyo by the strong hydrogen bond. Both the H-Obonds are 1. 21 Å in length. CNDO/2 calculation of charge density and Wiberg bond order for the compound yield the results consistent with the crystallographic data.
    The Crystal Structure of the Product from TNT with α,β-Unsaturated Aldehyde
    Chen Boren, Feng Zengguo, Liu Zuocai, Fan Guangyu, Cui Xiushan
    1990, 11(3):  305-306. 
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    3-Phenyl-5,7-dinitroquinoline-N-oxide is synthesized from 2,4,6-trinitrotoluene with cin-namaldehyde and its crystal structure has been determined by single crystal X-ray diffraction. The single crystal belongs to a triclinic system, P1 space group, a = 6. 637(3) Å, b = 7. 646(3) Å, c=13. 823(8)Å, a=75.81(4)% 3=77.63(4)° ,γ=88. 38(4)°,V = 666. 5(5) Å3. Z = 2. Least-square refinement has led to a final Rvalue of 0.045.
    The Syntheses and Properties of Substituted Semicarbazones and Thiosemicarbazones Containing Ferrocenyl Group
    Qiu Changlong, Zhang Yuhong, Zhang Xiucheng
    1990, 11(3):  307-309. 
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    This paper reports twelve new substituted semicavbazones and thiosemicarbazones which contain ferrocenyl group. All of these compounds are characterized on the basis of elemental analysis, IRand 1H NMR. Anumber of transition element (Cu, Co, Ni, Zn) complexes with thiosemicar-bazone prepared from formylferrcene and thiocarbohydrazide have been prepared and characterized. Using some of these compounds and Cu(Ⅱ) complexes, we have observed the bacteriostatic activity of them. It is shown that those compounds have significant bacteriostasis on Staphylococcus autreus, Bacillus Subtilis and Escherichia Coli.
    Aldol Condensation Catalyzed by the Transition Metal ( Ⅱ ) Coordination Compounds
    Zhang Yongmin, Xu Weillang
    1990, 11(3):  310-312. 
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    The aldol condensation of p- nitrobenzaldehyde with acetone catalyzed by metal ( Ⅱ )-ephedrine-BB-CDand metal ( Ⅱ )-N-methylephedrine-BB-CDsystems was carried out under mild and neutral conditions to afford an enantiomorphous excess aldol type product, 4-hydroxy-4-(4-nitro-phenyl)-2-butanone. The highest yield of the aldol type product is 82. 8%. The highest specific rotation [a]D15 is -6.7.
    Quantum Chemical Study of the Pharmacology of O-Ethyl-O-Aryl Phosphoramidothioates
    Han Yunzhu, Yang Guanghui, Zhao Chengda
    1990, 11(3):  313-315. 
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    The electronic structure of 14 O-ethyl-O-aryl phosphoramidothioates was studied by using a quantum chemical method of CNDO/2. The nucleophilic superdelocalizability on phosphorus and bond order of P-Oare found to show some linear relationship with experimental reactivity. Form the results, the pharmacology is suggeeested. The relationship of the pharmacodynamic conformation with the stable conformation is also discussed.
    Studies on Iron(Ⅲ) Heteropolytungstosillcates with M?ssbauer Spectra ( Ⅱ ) —Trisubstituted Heteropolytungstosilicate isomers
    Zhang Baojian, Qu Lunyu, Su Guifen, Li Zhongmin, Liu Shangui
    1990, 11(3):  316-318. 
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    The M?ssbauer spectra of the triferricononatungstosilicate isomers α and β-(Et4N)3.5Na2.5H-[SiW9Fe3(H2O)3O37] · xH2Owere determined. The Mossbauer parameters are as follows:δ=0. 198 mm · s-1, ΔEQ=0. 441 mm · s-1 for the α-isomer; δFea' = 0.190 mm · s-1Feb', = 0. 133 mm · s-1, ΔEQFea', = 1.197 mm · s-1, ΔEQFeb', = 0. 446 mm · s-1 for the β-isomer. The structures and bonds of the compounds were disscussed according to the Mdssbauer and XPSspectra as well as their magnetic moments. Both α and β isomers are all B-structure, which shows that A→Bstructure rearrangement occurred in the synthesizing process of the β-isomer.
    The Crystal and Molecular Structure of 2-Acetyl-3-Hydroxyestra-l,3,5(10)-Trien- 17-one(3a) and 2-Aceryl-Estra-l,3,5(10)-Trien-3, 170-Diol 17-Acetate(3b)
    Tang Zuohua, Xie Rugang, Duan Xiaofeng, Zhang Huabei
    1990, 11(3):  319-321. 
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    In this paper, 2-Acetyl-3-hydroxyestra-1,3,5(10)-trien-17-one (3a) ( Ⅰ ) and 2-Acetyl-estra-1,3,5 (10)-trien-3, 17BB-diol 17-acetate (3b) ( Ⅱ ) were synthesized, and their single crystals have were grown. The crystal structures of compound ( Ⅰ ) and ( Ⅱ ) were determined on the Nicolet four-circle diffractometer. Both compounds ( Ⅰ ) and ( Ⅱ ) belong to orthogonal crystal system. Crys-tallographicdata. ( Ⅰ ) space group C2221, a=10. 4361(29)Å, 6=11. 6299(36)Å, c=29. 2196 (107)Å. V = 3546. 41(1. 82) Å3, Z = 8; (Ⅱ ) space group p212121, a=7. 2312(21)Å, b = 12. 9008(50)Å, c=20.6798(75)Å, V=1929.16(75) Å3 Z=4. The rough molecular structures were obtained by the direct method. Refinement was carried out by the full-matrix least-square. The structures were refined to final R1 =0.0423 and R =0. 0368 for 1092 and 1625 observational reflections respectively. The results show that molecular inner-hydrogen bonds exist in both compounds ( Ⅰ ) and ( Ⅱ ). Ring Aof both compounds is planar and ring B, Cand Dare semi-chair, chair and envelope forms, respectively.
    Preparation and Characterization of Heteropoly Tungstotitanate Complexes of Lanthanide Elements
    Zhu Zhiping, Liu Jingfu, Zhao Benliang
    1990, 11(3):  322-324. 
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    The polytungstotitanates K13[Ln(TiW11O39)2] · xH2O (Ln = La, Ce, Pr, Nd, Sm, Eu) were prepared and analysed. Their IRand UVspectra, magnetic susceptibility and thermal stability were investigated.
    Synthesis and Properties of Poly(Silanacetylenes)
    Kan Chengyou, Wen Xiaoyao
    1990, 11(3):  325-327. 
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    The poly (diphenylsilanacetylene) ( Ⅰ ),poly (dimethylsilanacetylene) (Ⅱ ) and random copolymer of diphenylsilanacetylene and dimethylsilanacetylene ( Ⅲ ) were prepared via the condensation reaction between BrMgC≡CMgBr and R2SiCl2. The polymer can be dissolved in common organic solvents such as toluene,THF,and can be casted in films or drawn into fibers when melting except for ( Ⅲ ). The structures of polymers have been characterized by IR, 1H NMR, UVspectrometry and VPOmethods. The thermal stability and electroconductivity of these polymers were studied preliminarily.
    Study on the Kinetics of Polymerization by New Initiation Systems Copper Cu( Ⅲ ) Complex Ion ( Ⅰ ) —Polymerization of Acrylamide Initiated by Self-Reduction
    Liu Yinghai, Song Xingru, Shi Hongmei, Xu Lili
    1990, 11(3):  328-330. 
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    The kinetics of acrylamide polymerization initiated by potassium diperiodatocuprate (Ⅲ ) was studied in alkaline medium. The results indicate the equation of the polymerization rate is as follows: Rp=k[AM]1.8[Cu( Ⅲ )]0.76 and the molecular weight of a polymer decreases with increasing in Cu( Ⅲ). The effects of reaction conditions on polymerization rate were also studied.