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    24 July 1987, Volume 8 Issue 7
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    Articles
    Synthesis of the Rare Earth Coordination Compounds with Sulfamethoxypyridazine
    Gu Shangxiang, Deng Ruwen, Wu Jigui
    1987, 8(7):  575-579. 
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    In this work, the fifteen coordination compounds of rare earths with sulfa-methoxypyridazine were prepared in methanol medium. The compositions of the new coordination compounds were determined as LnA3·nCH3OH·mH2O(Ln= different rare earth ions, A=ion of sulfamethoxypyridazine), and their IRabsorption spectra,1HNMR spectra, TGcurves, X-ray powder diffraction, electric conductance and the solubilities in various solvents have been investigated, and their structures of coordination compounds were discussed.
    Studies on White Powdery Tungstic Acid(Ⅹ)--Ion Exchange Properties of white Powdery Tungstic Acid
    Zhu Sisan, Yang Yong, Gu Yidong(Yih-Tong Ku)
    1987, 8(7):  580-584. 
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    White powdery tungstic acid, which is considerably more active than yellow tungstic acid, was prepared under low acidity fay "the reversed way of acidification" in 1981, Aseries of compounds containing tungsten has thereby been prepared from the white powdery tungstic acid by virtue of the activities caused by the OHgroups connected directly to the tungsten atoms in the white powdery tungstic acid.The ion exchange properties of white and yellow powdery tungstic acids were therefore studied and used to compare their relative activities.In the method of Dynamic State, ion exchange capacities of both the tungstic acids were determined by use of exchange column, thereby the number of OHgroups connected with tungsten atoms were estimated. In the white powdery tungstic acid, isolated after two hours, digestion, about every two tungsten atoms are connected with one OH group, while about 25 tungsten atoms are connected to one active OH group only in the yellow tungstic acid.The more the ratio of OH group connected to the tungsten atom, the higher is the ion exchange capacity, and thus the more is the chemical activity.The ion exchange capacities of white powdery tungstic acid for several cation ions have also been studied by the method of shaking equilibrium (Method of Static State). The pHtitration curves of various tungstic acids have also been examined.
    Solubility Isotherms for the Quaternary System H3BO3-MgSO4-MgCl2-H2O at 273.15+0.05K
    Gao Zili, Gao Huade, Wu Bingli, Niu Yaozong, Yin Jingzhi
    1987, 8(7):  585-588. 
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    The quaternary system of H3BO3-MgSO4-MgCl2-H2O has been investigated at 273.15+0.05K by means of the isothermal method. This system is composed of three simple ternary systems:H3BO3-MgCl2-H2O (Ⅰ), H3BO3-MgSO4-H2O (Ⅱ) and MgCl3-MgSO4-H2O (Ⅲ). The solid phases identified are. (Ⅰ) H3BO3+MgCl2·6H3O;(Ⅱ) H3BO3+MgSO4·7H3O and (Ⅲ) MgCl2·6H2O+MgSO4·7H3O.There are three regions of the solid phases:H3BO3, MgCl2·6H2O and MgSO4· 7H2O in the central projection diagram. The eutectic point is at 33.44 Wt% MgCl2, 1.77% MgSO4and 0.65% H3BO3.
    Determination of Some Basic Constants of Extractant P229
    Chen Jinbang, Liao Qimu
    1987, 8(7):  589-591. 
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    In this paper some basic constants of extractant di(2-ethylhexyl)-phosphinic acid (P229) were determined. The solubility (S) of P229 in water was determined by the conductometric and pH methods. The ionization constant (Kα) of P229 in aqueous solution, distribution constant (Kd) and dissociation constant (Kαe) of P229 between octanol-water two phases were determined by two phases titration method. The results are as follows. 5=4.64×10-5mol·dm-3, pKα= 4.58, pKαe= 8.50, lgKd=3.92 (25±0.2℃).
    Studies on Potentiometric Stripping Analysis with a Hanging Mercury Dropping Electrode
    Ruan Xiangyuan, Zhou Duanci
    1987, 8(7):  592-594. 
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    Equations describing the potentiometric stripping analysis (PSA) with a hanging mercury dropping electrode (HMDE) are deduced. Transition time equation and E-t curve equation are obtained and quantitative relationship between transition time and parameters, e.g., the cocentrations of determined ions and oxidant preconcentration time, electrode radium, etc, is also obtained. All the theoretic conclusions were verified experimentally, and the results are in agreement with the theory.
    Studies on Adsorption Potential Stripping Analysis
    Bai Yan, Zhou Duanci(Chau Tuanci)
    1987, 8(7):  596-600. 
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    The potential stripping behaviour of Cu(Ⅱ) and Sn(Ⅳ) in cysteine solution was studied in detail. Sensitivities for the analyses by APSof the two elements in this system may be increased by 1-2 orders of magnitude under optimum conditions (forCu(Ⅱ):0.50M NaCl, pH3.0, 2×10-4M GysH, Ed-0.90V; for Sn(Ⅳ): 0.40M NaNO3, pH2.9, 3×10-4M CysH, Ed-l.10V), with the variation coefficients 2.6% and 1.4% separately.It was observed that with co-existance of Cu(Ⅱ), cysteine also gave well-defined potential stripping waves which may be used to determine cysteins. Uader optimum conditions (0.50M NaNO3, pH2.8, 1×10-5M Cu(Ⅱ), oxidate. Hg(Ⅱ),the transient time(τ) is proportional to cysteine concentration in the range of 2×10-10-1×10-5M, with the variation coefficient 2.5%.
    Solvation Effects on Colour Reactions of Fluorescent Complex--Gallium (Ⅲ) -Morin-Aqueous Solvents System
    Wang Huaigong, Li Lanyun
    1987, 8(7):  601-603. 
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    Solvation effects of aqueous organic solvents on complexes of Gallium (Ⅲ)-Morin have been investigated by us firstly. It has been proved that in the presence of organic solvents, the sensitivity and selectivity of fluorescent reaction are greatly increased. The fluorescent yield of the solvated complex Ga(Ⅲ)-Morin-MeOH is 0.505. Ahighly sensitive method for the determination of trace Gallium was recommended. The interference of foreign ions was studied. Satisfactory results were obtained in the determination of trace Gallium in pure Berillium and pure Indium. The composition, fluorescent yield, molar absorptivity were measured.
    Maximum Likelihood Estimation Method and Its Application to Potentiometric Titration of Acid Mixtures
    Luo Guoan, Wang Baojun
    1987, 8(7):  604-609. 
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    Aformula for the calculation of the equivalent volume of acid mixture titration is derived. Within this formula the measured value of the hydrogen - iois expressed by activity. Anonlinear model parameter estimation methodmaximum likelihood estimation method (MLE) is presented. It takes into account the different errors in pHand V (vol.) data obtained from the determination of the mixture of acids. It gives out more satisfactory results than that obtained from the least squares estimation method (LS). The Monte Carlo method has been employed to the study of the results obtained from methods of MLEand LS.
    Study on Cobalt-Carbon Cluster--Synthesis of α-Naphthyl, α-Thienyl and Substituted-Phenyl Phenylacetylene Dicobalt Hexacarbonyls
    Song Licheng, Wang Zhongxia, Wang Jitao
    1987, 8(7):  610-614. 
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    12 New diarylacetylenedicobalt hexacarbonyl complexes have been synthesized by complexation reaction of α-naphthyl, α-thienyl or substituled-phenyl phenylace-tylene with Co2(CO)8and N-acetylalion of p-aminophenyl phenylacetylenedicobalt hexacarbonyl. The structures of all the complexes were characterized by elemental analysis, IRand 1HNMR spectroscopy. Through comparison of N-acetylation of p-aminophenyl phenylacetylenedicobalt hexacarbonyl and aniline under comparable conditions, it was found that the cluster core PhC2Co2(CO)6para to an amino group attached to aromatic ring does not obviously affect the nucleophilicily of aniline.
    Synthesis of 2-Substituted-1,1,1-Trichloro-3-Nitropropane
    Chen Qijie, Liu Fengping, Xie Longguan
    1987, 8(7):  615-619. 
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    The syntheses of fourty-six 2-hydroxy-,2-amino-, 2-hydrazino- and 2-ni-trogenous heterocyclyl-1,1, 1-trichloro-3-nitropropane derivatives were described. Preliminary bioassays showed that the compounds exhibited fairly good fungistatic activity, among them 2-phenylhydrazino-1, 1, 1-trichloro-3-nitropropane is the most effective.
    Synthesis of Piscidic Acid and Its Epimer
    Nie Xinyong, Wang Qian, Li Yulin, Pan Xinfu
    1987, 8(7):  620-622. 
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    The (2R,3R) -dimethyl tartrate acetonide(1) was reacted with p-benzyloxy-benzyl bromide(2) at-78℃ in the presence of LDAto convert successfully(1) to dimethyl(2R,3R)-2-benzyloxybenzyl-tartrate acetonide (3). The dimethyl (2R, 3R)-2-benzyloxybenzyl-tartrate acetonide (3) was treated with CH3ONa and the major product was the 81% enantiomerically pure erythro-isomer (5). The benzyl and acetonide groups of dimethyl (2R,3S)-2-benzyloxybenzyl tartrate acetonide (5) and dimethyl (2R,3R)-2-benzyloxybenzyl tartrate acetonite (3) were removed, respectively, by treating with CH3CO2H-HCl-H,O(2:1:1) for 1.5 hrs., and hydrolyzing with 0.5N NaOH. The piscidic acid (8) and its epimer (7) were obtained successfully.
    Photochemical Reaction of Ferrocene-Tetracyanoethylene Complexes
    Meng Jiben, Matsuura T.
    1987, 8(7):  623-625. 
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    Photochemical reaction of ferrocene-tetracyanoethylene (Fc-TCNE) complexes has been investigated. The photochemistry of (Fc-TCNE) in the solid-state is. distinct from that in solution. While only cyanoferrocene (F1) was obtained when the reaction was carried out in solution, both cyanoferrocene (F1) and 1,2-diferrocenyl-1,1,2,2-tetracyanoethane (F2) were obtained when it was carried out in the solid-state.
    Studies on the Synthesis and Properties of β-(N-Arylamide)Ethyl Germanium Sesquioxides
    Bai Mingzhang, Yang Shujun, Sun Lijuan, Wang Shixian, Wang Jie
    1987, 8(7):  626-628. 
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    Fifteen new compounds of (GeCH3CH2CONHAr)2O3type were prepared. Elemental analysis and IRspectrum determination have been carried out for all of these compounds. Antitumour activity was determined as well.
    Study of the Crystal Structures of Silatranes (这里有图片198707-634-1.gif)
    Lin Xiuyun. Zheng Qitai, Wu Shen, Zhang Shude, Shen Fuling, Wang Jitao, Xie Qinglan, Liao Renan, Li Jing
    1987, 8(7):  629-634. 
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    Silatrane Ibelongs to monoclinic system with space group P21/N(Z=4) and silatrane Ⅱ belongs to orthorhombic system with space group Pcab(Z= 8).The lattice parameters are.Ⅰ,α= 11.876(2)Å, 6=19.853(4)Å, c= 6.598(1)Å, β=110.12(2) Ⅱ.α= 19.653(4)Å, b=12.565(3)Å, c=12.570(3)Å.The structures were solved by RANTAN and refined by Full Matrix Least-Square Method. The final R-factors are 0.09 and 0.06, respectively.The N→Si bond of silatrane Iis shorter than that of Iand both of them are shorter than those of other kinds of silatranes.
    Infrared Study on Interaction Between Methacrolein and Catalyst H4PMo11V1O40/SiO2
    Wu Tonghao, Yang Hongmao, Want Guojia
    1987, 8(7):  635-639. 
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    In this paper, we reported the result of infrared study about methacrolein (MAL) adsorption on heteropoly acid catalyst, H4PMo11V1O40/SiO2.The three surface species CH2=C(CH3)-CHO(Ⅰ), CH2=C(CH3)-CO (Ⅱ) and(这里有图片198707-639-3.gif)(Ⅲ) were formed on the catalyst surface. We considerthat they are the intermediate compounds of methacrylic acid (MAA) to form. It was found that at 300℃ MAL chemisorption did not occur on the catalyst under the evacuating condition. VP-Oand VMe-O-Mebands, characterizing the heteropoly acid anion structure, disappeared.
    A Study of Infrared Absorption Spectra and the Mechanism of the Decomposition on the Bis-Thiourea Gold (Ⅰ) Complex
    Wang Qinhe, Lou Yongqin, Lu Dajun, Shao Jingren, He Yuanlong
    1987, 8(7):  640-644. 
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    Infrared spectra, differential thermal analysis curves and thermogravimetry curves of the bis-thiourea gold (Ⅰ) complex have been measured. In the heating process of the complex, the infrared spectra of the solid products of heat decomposition of the complex at 21 different selected temperatures have been measured, and the mechanism of heat decomposition was infered. The apparent activation energy and the preexponential constant of heat decomposition reaction were evaluated. At the heating rate of 10℃/min and in the range 230-260℃, thiou-rea in the ligand isomerizes into isoammonium thiocyanate. The decomposition of complex starts at 240℃ and ends at 322℃. Au2S decomposes into the metal Au above 650℃.
    A Study of GLPC Method for Determination of the Activity Coefficients of the Volatile Components in Binary System
    He Jiajun, Li Fuhua, Huang Zhongliang
    1987, 8(7):  645-647. 
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    Based on Chueh-Ziegler method, a regular experimental process and a new formula for calculating activity coefficients from GLPC data are pressented. With this new method, activity coefficients of benzene in benzene (φH)-dinonyl phthalate (DNP) system at 50°, 65°, 80°and 95°are determined and given good results.
    Monte Carlo Simulation of Binary Gopolymerization(Ⅰ)--Terminal Model and Sequence Distributions of Copolymers
    Yang Xueshi, Yan Juntan
    1987, 8(7):  648-652. 
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    A BASICprogramm of Monte Carlo Simulation of binary copolymerization was made according to the Terminal Model.The number of Runs of the two units of the copolymer chain formed is counted along with the simulation. Results obtained by this programm are very close to those calculated by using first order Markov chain. This programm can be used in studies of sequence distributions of binary copolymers formed by terminal model.
    Synthesis of Some New Polymeric Ligand-Anchored Rhodium Catalysts and Their Hydroformylation Properties
    Sun Juntan, Weng Junfan, Li Hong, He Binglin
    1987, 8(7):  653-657. 
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    Several new types of polymeric ligand and the corresponding rhodium complexes, were synthesized using crosslinked polystyrene as the parent support. The catalytic properties of the catalvsts for the hydroformylation of diisobutylene and pentene-1 were investigated. The loss of rhodium of the catalysts was observed.
    Synthesis and Application of Poly(EthyleneOxide)Macromers(Ⅱ)--Preparation of Polyacrylic Acid-g-Polyethylene Oxide Copolymer Based on Polyethylene Oxide Macromer Capped with Allyl Group
    Sua Fang, Wang Mang, Zhu Hongjun, Yang Shilin(Ping Lum Ho)
    1987, 8(7):  658-663. 
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    Copolymerization of allyl group-capped PEOmacromers with acrylic acid co-monomer to obtain a new type of graft copolymer(PAA-g-PEO) was reported. With the help of model test it is illustrated that the obtained polymer is of the expected structure. A method to determine the composition of copolymer based on IRspectrometry has been set up. Several effects on the copolymerization were examined and the specific solution-behavior was also reported.
    Studies on the Copolymerization of Propylene and Butadiene with Supported Titanium Catalysts (Ⅰ)--Copolymerization and Characterization of the Products
    Wu Qing, Lu Zejian, Lu Yun, Lin Shangan
    1987, 8(7):  664-669. 
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    Propylene-butadiene copolymerizations with TiCl4/MgCl2/AlEt3and TiCl4/ MgCl3/AlEt3/EB catalyst were studied respectively. It was found that copolymer obtained by the first catalyst give more butadiene content and lower reduced viscosity than that obtained by second one. The copolymerization products have been confirmed to be copolymer containing long propylene-propylene sequence and butadiene-butadiene sequence by solvent extraction, IR, 13CNMR, X-ray, and DTA. Butadiene unit in copolymers is exclusively in trans-1,4 structure.
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