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    24 March 1987, Volume 8 Issue 3
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    Articles
    Complexes of Crown Ether with the Rare Earth Nitrates (ⅩⅥ)--Synthesis and Characterization of Complexes RE(NO3)3·B12C4·xH2O
    Jiang Haiying, Song Disheng, Lu Yugang, Yan linying, Li Xiuzhen, Zhu Zhenhua, An Youzhen
    1987, 8(3):  193-198. 
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    The complexes of the rare earth nitrates with benzo-12-crown-4 were synthesized in CH3CH or CH3COCH3All of the complexes RE(NO3)3·Bl2C4.xH2O (where RE=Pr, x=2; RE=Nd, x =0; RE=Y, Tm, Yb, Lu, x=3) were formed in the solid state. They were characterized by spectrophotometry, chemical analysis, infrared spectra, U. V. spectra, X-ray diffraction, chromatography of gases, thermogravimetric and differential thermal analyses. Besides, the solubilities of the complexes in CH3CN were determined at 15±0.1℃.
    Studies on Complexes of Rare Earths with Crown Ethers (Ⅺ)--Synthesis and Characterization of the Complexes of Scandium and Yttrium Nitrates with Dibenzo-24-Crown-8
    Qi Youxun, Tan Minyu, Zhai Yingli
    1987, 8(3):  199-203. 
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    The solid complexes of scandium and yttrium nitrates with dibenzo-24-crown-8(DB24C8), having the compositions Sc(NO3)3·DB24C8· 2H2O and [Y(NO3)3]4·(DB24C8)3·8H2O, were synthesized in acetonitrile medium and characterized by elemental analyses, JRand UVspectra, thermogravimetric (TG) and differential thermal analyses and X-ray powder diffraction.
    Disulf oxide Complexes of Europium Perchlorate
    Zhang RuoHua, Xue Qunshan
    1987, 8(3):  204-208. 
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    The synthesis and characterization of the complexes between Eu(ClO4)3and bis (n-octasulfinyl) ethane and bis(phenylsulfinyl) ethane of high-melting (α) and low-melting (β) isomers are reported. The composition of compl exes of two isomers is rot the same. The complexes are Eu(ClO4)3·(α-BOSE)3·2H2O, Eu(ClO4)3·(β-ECSE)4·2H3O, Eu (ClO4)3·(α-BPhSE)3and Eu(ClO4)3·β(-BhSE)4·2H2O.Eu(Ⅲ) ion are bonded to disulfoxide group and perchlorate ion via the oxygen atoms. The absorption bands of f-f transition of metal ion, charge transition of metal←ligand and electronic transition of ligand were observed. Emission spectra of complexes were also determined.
    Synthesis of Two Series Arsenazo Types with Different Auxochromic Groups and Positions and Studies on Their Colour Reactions for Rare Earth, Thorium,Zirconium and Uranium
    Dai Pingqi, Yu Ximao, Luo Qingyao, Zeng Yun'e
    1987, 8(3):  209-214. 
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    In this paper, two series of arsenazo types reagents with diffrent auxochromic groups and positions for rare earth, thorium etc. have been designed and synthesized. The reagents were purified by TLCand their strutures were determined by infrared spectra, quantitative elemenitary analysis and thermogravimetrici analysis. They are easily soluble in water, alcohol and acetone but insoluble in benzene and ether. The colour reaction of the reagents with rare earth, thorium and zirconium elemnts have also been studied. The result shows that the effects of their molecular structure on the colour reaction have some regularity. The absorption maxima of the complexes of reagents o-As-TX (X=C1, Br,I) with La, Gd, Yb gradually increase with the dercrease in electronegativity of subtituent Gl, Br, I, but with Y, the phenomenon is contrary. The sensitivity of o-As-DXN reacting with rare earth elements are lower and rapidly decreases with the increase in acidity of medium, but with Th, Zr, it is still higher. In these colour reagents, o-As-DBNis excellent colour reagent in the determination of thorium The tolerant quantity of rare earth elements can reach several milligrams, especially for uranium.
    Investigation on the Concentration of Pollution Matters in Birds at Different Environmental Conditions (Ⅰ)--Application of inductively Coupled Plasma-Atomic Emission Spectrometry to Simultaneous Determination of Ca, Na,Mg, P, Fe, Al, Cu, Mn, Cr
    Jiang Zucheng, Cheng Zhujun, Hu Hongxing, Li Bailian, Wang Yuanxiang
    1987, 8(3):  215-220. 
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    A method for the determination of Ca, Na, Mg, P, Fe, Al, Cu, Mn, Cr and Zn in the bird eggs by using ICP-AESis described in this paper. The optimum experimental conditions of ICPdischarge were selected; the effects of coexistent elements(Ca, Na, Mg) on line intensities of the analyte and the methods of sample digestion were discussed. The normal concentrations and their contributions in the eggs of Passer montanus saturatus, Ardeola bacchus, Egretta garzetta, nycticorax nycticorax, Pigeon and Hen were also reported. Under experimental conditions the detection limits for the analyte are 0.0029-2.5μg/ml, the relative standard deviations are in the range of 1.3 to 4.6%, and the recoveries of the method are 90-115%.
    Improvement in Sensitivity of Spectrophotometric Method of Antimon-Heteropolymolybdic Acid by Ethyl Alcohol and Its Application to Arsenic Analysis
    Sun Ting, Wang Bing-wu
    1987, 8(3):  221-225. 
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    A sensitive spectrophotometric method for arsenic analysis is described. The higher sensitivity comes from the effect of ethyl alcohol on the reduction reaction of antimon-heteropolymolybdic acid. The sensitivity of this method is 50 times higher than the normal arsenoantimonomolybdate method. The detection limit(based on three times the standard deviation of ten blank measurment) is 18ppt (50ml water sample) and the coefficient of variation is 0.8% and 3.8% at the blank solution and the 0. 3 μg level, respectively.The effect of ethyl alcohol is discussed preliminarily. The reduction reaction of antimon-heteropolymolybdic acid was catalyzed by As(Ⅴ) only when ethyl alcohol or other organic solvents (in water) such as methyl alcohol, isopropanal, dimethylformamide, dioxane and ice acetic acid exists in the arsenoheteropolymo-lybdate solution.
    Photochemical Reaction to the Application of Analytical Chemistry--Determination of Copper(Ⅱ) Based on Its Inhibitory Effect
    Liu Shibin, Men Ruizhi, Piao Tiehua
    1987, 8(3):  226-228. 
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    Copper(Ⅱ) can effectively inhibit the photo-induced reaction of I2formation. Since there exists a quantitative relationship between irradiated time to the end-point versus concentration of copper(Ⅱ), therefore copper (Ⅱ) contained in samples can be quantitatively determined.The optimal experimental conditions have been examined. The interference behaviour of about 20 foreign ions were observed. This new method for the determination of micro-copper (Ⅱ) has been used in the analysis of tap water, lake water and cabbage samples and satisfactory result was obtained.The end-point was determined by "die-stop titration" method. The data were processed with a micro-computer,using a program written for lagrange's interpolation formula fitting to the nonlinear calibration curve.
    Studies on the Acylthiosemicarbazides and Their Related Heterocyclic Compounds (Ⅳ)--Studies of 1-Cyanoacety 1-4-aryl Thiosemicarbazides and Their 1,2,4 -triazoline-5-thione Derivative
    Zhang Ziyi, Chen Limin, Feng Xiaoming, Du Youngkan
    1987, 8(3):  229-234. 
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    In this paper a series of new 1-cyanoacetyl-4-aryl thiosemicarbazides (Ⅰ) have been synthesized. When aroylisothiocyanate reacted with 1-cyanoacetylhydra-zine in acetonitrile or acetone, the corresponding compound (Ⅰ) was formed respectively in yield of about 50-95%. Promoting effects of compounds (Ⅰ) on growth of plant have been tested preliminary.Compounds (Ⅰ) may be cyclized in the presence of 2N K2CO3aqueous solution to give 1,2,4-friazoline-5-thione derivatives (Ⅱ) in fairly good yield (70-90%).
    Studies on Steromers of Triadimenol (Ⅱ)
    Li Zhengming, Dong Lixia, Li Guowei, Zhang Zuxin, Cao Qiuwen, Wang Suha, Dou Shiqi
    1987, 8(3):  235-239. 
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    The two diastereomers ( designated as Aand B ) of Triadimenol were separated and the enantiomers of the active triadimenol Awere further resolved. The absolute configuration of (+)-triadimenol Awas determined both by Horeau method and X-ray diffraction method. Its oxidation to the corresponding (+)-triadimefon was successfully carried out for the first time by Jones' oxidation. The asymmetric reduction of (+)triadimefon was carried out by using an hydrogen transfer mechanism of Grignard reaction to obtain different optical isomers of triadimenol.The preliminary bioassay on mixed spores of wheat rust indicated that among the four optical isomers of triadimenol, (-)-A-lS,2Renantiomer has the highest bioactivity, whereas both levo- and dextro- isomers of triadimefon do not differ much in their bioactivities.
    Preparation of Ethers Through Phase Transfer Catalysis
    Chen Jichou, Dai Yujia, Wang Lanfang, Niu Junkai, Chen Shufen
    1987, 8(3):  240-242. 
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    Twenty-two ethers have been synthesized by means of liquid-liquid and solid-liquid phase transfer catalysis. In comparison with original Williamson's method, the present procedure has the advantages of high yield and simplicity in operation.
    Synthesis and Catalysis of Bicyclo[2,2,1]hept-5-ene-2-methoxy and-2-Carboxytitanocene
    Ma Yongxiang, Hou Xue, Man Huaqing
    1987, 8(3):  243-245. 
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    (这里有图片198703-245-1.gif) These compounds caninitiate radical polymerization of acrylonitrile on illumination.
    Synthesis of Benzalchloroimine-1-d by Umpolung and Catalytic Decomposition of Benzalchloroimine
    Zhang Jingliu
    1987, 8(3):  246-248. 
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    This paper reports a simple preparative method of benzalchloroimine-1-d. The kinetic study on the reaction of benzalchloroimine Ia-b with diphenyl sulfide in benzene has been carried out. From, p value of Hammett equation and the kinetic isotope effect, its mechanism of reaction was tendered.
    The Regularity About the Effect of the Promoter P2O6on the Activity of Vanadium Pentoxide Catalyst
    Yu Qingrei, Zheng Xiaoming, Jin Shongshou
    1987, 8(3):  249-254. 
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    Under the direction of the theory of the corresponding group structure of the catalyst, we advanced the theory model to clarify the oxidation activity of the catalyst. The model has been proved by our experiments to be reasonable.We used it to explain numerous experiment facts that can not be answered by previous oxidation activity concept and to draw some clear conclusions.
    Studies on Natural-Abundance Nitrogen-15 Nuclear Magnetic Resonance Spectroscopy (Ⅰ)--Long-Range Interaction on Nitrogen-15 Chemical Shifts of 4-Substituted Piperidines and Their Correlation with Carbon-is Chemical Shifts
    Yang Li, Liu Peiqi, Kong Suling, Dong Ying, Chen Yaozu
    1987, 8(3):  255-259. 
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    Natural-abundance 15N and 13CNMR chemical shifts of eight 4-substituted 2,2,6,6-tetramethylpiperidines have been measured. It is found that the 15N chemical shift is correlated with the electronegativity of the 4-substituent, indicating a long-range interaction of the 4-substituent on the 15N chemical shift. Alinear relationship is also present between the 13C chemical shifts and the electronegativity of the 4-substituted atoms.
    Quantum-Chemical Calculations(PPP Method) of Some Properties of Organic Reagents
    Li Menglong, Zhang Kaicheng
    1987, 8(3):  260-264. 
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    Acomputer program of PPPmethod for the electronic structures and spectroscopic properties of organic reagents has been prepared. Pyridyl azo reagent series have been studied with this program. The wave-long absorption spectra of some organic reagents determined by our experiments were compared with the calculated results and a good agreement was found.
    Program for Spectral Analysis of NMR AA' BB' Proton System
    Zhou Zheren
    1987, 8(3):  265-267. 
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    A computer program for spectral analysis of NMR AA'BB' proton system is presented for routine application. The problems to simplify calculations in applying group theory method, to acquire spectral parameters and recognize the origin of every spectral line by the use of sub-spectral method are discussed.
    Study of the Activity Coefficient of TBP-TTA-C6H6Multicomponent System
    Zhong Yunxiao, Xiao Bo, Pen We, Pen Qixiu
    1987, 8(3):  268-270. 
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    For the investigation of the binary synergic extracting regularity, a multico-mponent system TBP-TTA-C6H6were studied. The activity coefficients of benzene and tributylphosphate (TBP) were measured by vapour pressure and 32P-labeled TBPdistribution method respectively, then the activity coefficient of thenoyltri-fluroacetone (TTA) was obtained by Gibbs-Duhem equation. The activity coefficient of benzene, which dissolved two solutes-TBP and TTA simultaneously, have been also calculated by statistical theory using cluster expension method. The result is consistent with experimental data in the region of mole fraction of benzene greater than 0.6.
    Research Thermal Decomposition of Lanthanum Hydroxide by Thermogravimetry
    Cui Shengfan, Yang Wensheng, Qiao Zhengnan
    1987, 8(3):  271-272. 
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    Thermal decomposition of lanthanum hydroxide proceed in two step, the first step lose two molecules of water and the second step lose one molecule of water, activation energy of these reaction are equal to 16.9 kcal/mol and 43.0 kcal/mol respectively.
    The Glass Transition Temperature and Liquid 1-Liquid2Relaxation of Star-Shaped Polystyrene
    Wang Jian, Liu Jingjiang, Yang Meilin, Shen Jiacong
    1987, 8(3):  273-276. 
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    The glass transition temperature Tgand T11relaxation of a series of regular star-shaped polystyrenes were measured by tortional braid analyzer(TBA) and linear dilatometer. The results show that the Tgof star-shaped polymer increases with increasing branching degree when the molecular weights of branch chains are the same, but it is lower than that of linear polystyrene of the same molecular weight. The liquid1-liquid2relaxation temperatue T11and the strength of loss peak of star polystyrene also depend on branching degree. Two-Tgtransitions in star polystyrenes with DVBmicrogel nodule were proved by comparing two type of star polystyrenes.
    The Formation of Cation-Complex DNA Studied by Laser Scattering (Ⅱ)
    Zuo Ju, Zhang Min, Yang Yingsong
    1987, 8(3):  277-282. 
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    The kinetics and the influence factors of complex precipitation of DNA with Mn++, Ni++and Cu++were studied by the laser scattering. The influence factors are M/P, concentration, pHand t(℃) etc. The experiments obtaining the active energies of the reaction, the complex ratio and the reaction order were also done. And the active order which was derived from active energies for complex precipitation is Mn++<Ni++<Cu++, which is accord with the result from CFT. The presence of small ions Na+, K+, etc. plays, indeed, a important role in the formation of complex precipitation. The mechanism of complex precipitation was also analysed.
    Synthesis of Some New Fluoro-Organosilicon Compounds
    Chen Jianhua, Zhang Chengzhi, Du Zuodong
    1987, 8(3):  283-287. 
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    The additions of organosilicon compounds containing Si-H bonds to 2,2,3,3-tetrafluoropropyl allyl ether are studied. Aseries of unreported organosilicon com-pounds have been synthesized. The method of synthesis of 2, 2, 3, 3-tetrafluo-ropropyl allyl ether is improved. Some works on organosiliconpolymers containing fluorine are reported.
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