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Table of Content

    24 January 1987, Volume 8 Issue 1
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    Articles
    Studies on Ternary Complexes of Cobalt (Ⅱ) Containing Iminodiacetic Acid and Some α-Amino Acids
    Fan Chunmei, Zhang Jia
    1987, 8(1):  1-4. 
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    The stability constants of ternary complexes of Co(Ⅱ) with iminodiacctic acid (IDA) as the primary ligand and glycine (Gly),Alaninc (Ala), Nor-Valine (Nor-Val),phenyl-alanine (Phc),methionine (Met),Serine (Ser),asparagine (Asn) as the secondary ligand have been determined.Auxiliary data,such as the acid dissociation constants and the binary stability constants of Co(Ⅱ)-IDA and Co(Ⅱ)-Met,have also been obtained under identical conditions. The stability of the ternary complexes and the coordination manner of some potential tridcntate ligands have been discussed in terms of their stability-constant data.
    Studies on Thermodynamic Properties of Crown Coordination Compounds (Ⅷ)--The Coordination Reaction of Methyl Benzo-18-Crown-6 Derivates with Some Alkali Metal Ions Studied by NMR Method
    Luo Qinhui, Li Chongde, Feng Xudong, Wei Jinhua, Hu Hongwen, Dai Anbang
    1987, 8(1):  5-11. 
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    Thecoordination reaction of alkali metal ions with methyl Benzo-18-Crown-6 derivates containing 1-3 methyl groups on their crown ring was studied by 13CNMR method, which gives the information about the conformation of the complexes in solution.The electric charge density of carbon atoms on the crown ring was calculated by CNDO/2 method and a linear relationship between electric charge density and corresponding chemical shift was found.The stability constants of Na+-crown complexes were determined by 23NaNMR,showing also a linear relationship with the number of methyl groups on the crown ring. lgβ= 4.16-0.20n wherein n denotes the number of methyl groups.
    Studies on Two N-Heterocyclic Hydroborates and Their Complexes
    Zhang Lun, Fang Xinqin, Zhu Weiming
    1987, 8(1):  12-16. 
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    Two novel ligands, potassium monohydrotris(1-imidazolyl) borate and potassium dihydrobis(l-bcnzotriazoly])borate have been synthesized via the molten reactions of potassium borohydride with imidazole or benzotriazole, these have been identified by MS, 1HNMR, elemental analysis and IRspectra. Their complexes with Co(Ⅱ), Ni(Ⅱ), Cu(Ⅱ),and Zn(Ⅱ) were described.
    Studies on Solid Metal Complexes of o-Hydroxybenzyl-Amine (HBA) with Cu(Ⅱ), Fe(Ⅲ)
    Zhang Huinong, Zheng Peiju, Yang Hongping, Zhang Hualin
    1987, 8(1):  17-21. 
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    The complexes of o-hydroxybenzyl-amine (HBA) with Cu(Ⅱ), Fe(Ⅲ) have been prepared in solid state and characterized by elemental analyses, infrared spectra, thermogravimetric, solubility, molar conductance, magnetic moment and sing-lecrystal X-ray diffraction. The complexes formed are proved to be green Cu(HBA)2·1.5H3O, brown Cu(HBA)2and brownish red Fe(HBA)3.
    Studies on Preparation and Characterization of Coordination Compounds of Rare Earths with Solapsone
    Ma Xianxian, Wu Jigui, Deng Ruwen, Song Chaojie
    1987, 8(1):  22-24. 
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    The fifteen coordination compounds of rare earths with solapsonc, with the exception of Pm solapsone salt, were synthesized by the reaction of RECl3with solapsone in methanol medium. The composition of these coordination compounds has been determined as RE4(PS)5·5H2O. Their IRabsorption spectra, UVabsorption spectra, TGcurves, electric conductance and the solubilities in different solvents have been investigated and characterized.
    Atomic Absorption Spectrophotometric Studies on Rare Earth Elements (Ⅲ)--The Relation between the Structural Factors of Organic Complexing Agents and the Enhancement Effect
    Wu Dehuai, Zhou Chiming, Wang Jianyan, Liu Mingxia
    1987, 8(1):  25-30. 
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    The influence of the structural factors (the type of complcxing agents, the kind and the number of bonding atoms and their relative position, the conjugated system and its size, the formation of chelate ring and the molecule with or without sulfonic acid group) of organic complexing agents on the enhancement effect of ytterbium was studied in an air-acetylene flame. The rule and the mechanism of the enhancement effect were discussed. The results indicate that the kind of bonding atom is a important factor deciding enhancement OT suppression action of complex-ing agent and the information obtained should be a comprehensive result affected by all these factors cooperatively in this case.
    The Spectrometric Determination of p-Aminoazobenzene and Its Chlorides
    Huang Yongnian, Ge Xiaoxin, Wang Yiqing, Qi Deyao
    1987, 8(1):  31-32. 
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    The method is based on the reaction of sodium sulfide and formaldehyde with the determined compound in hydrochloric acid solution,forming a purplish-red colour solution. It was measured at λmax515 nm by spectrophotometry.
    Dual-Wavelength Spectrophotometric Determination of Nitrate and Nitrite with 2,6-Xvlenol
    Zhang Youxian, Pan Liying, Zhao Min, Gao Waling
    1987, 8(1):  33-35. 
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    Nitrate and nitrite react with 2,6-xylenol in H2SO4solution. On the basis of this fact we simutaneously determined nitrate and nitrite with dual-wavelength at 318nm-290.5nm and 305.5nm-332.5nm. Beer's law is obeyed in the range 0.00-19.03μg NO3--N/25ml and 0.00-12. 00μg NO2--N/25ml and △ε318;390.5nm is 2.3×103and △ε305,332.5nm is 4.74×103. After neutralization of solution with NaOH, spectra took place bathochromic shift and nitrate and nitrite can be determined with dual-wavelength at 417.5nm-359nm and 384nm-463.5nm. Beer's law is obeyed in the range 0.00-7.61μg NO3--N/25ml and 0.00-4.8μg NO3--N/25ml and △ε417.5,359nm is 1.13×104and △ε384,463.5nm is 1.29×104This methed was applied to determine of nitrate and nitrite in water.
    The Synthesis and Anticonvulsant Activity of Some α-Halo-m-Trifluoromethyl Cinnamamides
    Ling Yangzhi, Xu Yanna, Li Anliang, Liu Weiqin
    1987, 8(1):  36-40. 
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    Nine α-halo-m-trifluoromethyl cinnamides were synthesi2ed from trjfluoro-methyl benzene, via bromination, Grignard reaction, condensation, halogen addition reactions etc, as indicated in the synthetic scheme. Their configurations were confirmed by NMR. Their pharmacological results showed that, the introduction of α-halogen group, did not enhance their anticonvulsant activity as expected.
    Asymmetric Induction (Ⅰ) Addition of Chloroform to Benzaldehyde in the Presence of Chiral Ammonium Salts
    Shi Yaoceng, Pan You, Hu Hongwen
    1987, 8(1):  41-46. 
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    The chiral ammonium salts have been used as phase transfer catalysts for asymmetric synthesis. The addition of chloroform to benzaldehyde in the presence of chiral ammonium salts, quinine, N-benzyl-quininium chloride (BQC), N-benzyl-dihydroquininium (BDHQC), N-(o-nitrobenzyl) quininium chloride (NBQC), N-benzylquinidinium chloride (BQDC), N-benzylcinchonium chloride (BCDC), N-dodecylquininium bromide (DQB), quinine-acrylonitride copolymer (QN-AN), N-benzyl quininium chloride-acrylonitride copolymer (QNBC-AN) and N-benzyl-N-methylephedrinium chloride (BMEC) is reported. The effects on the optical yields, such as (Ⅰ) the solvent effect (Ⅱ) the amount of catalysts (Ⅲ) the time of reaction and the Induction machanism are studied.
    Studies on the Kinetics of Decomposition of Diacyl Peroxides (Ⅷ) --CIDNP Effect of the Products of Thermolysis of Octanoyl Peroxide and Hexanoyl Peroxide
    Liu Youcheng, Guo Qingxiang, Liu Peiqi
    1987, 8(1):  47-51. 
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    1H ClDNP spectra recorded during the decomposition of aliphatic diacyl peroxides [(RCOO)2, R = n-C7H15(1), n-C5H11(2)] in ODCB in the presence of scavengers, such as I2, C2H5I,(CH3)2CHI, and CH2=CHCH3Br, show multiplet effect polarization for RX (X= Br, I) and disproportionate products, R-H. The reaction mechanism is discussed in terms of radical pair theory.
    Research on 2-(ω-Biphenylyl)Polymethylene-5-BiphenyIyl-Oxazole-1,3 and 2-(ω-Biphenylyl)Poylmethylene-5-Biphenylyl Oxadiazole-1,3,4
    Zhou Yimin, Xiao Changhe, Wang Shenxiu
    1987, 8(1):  52-54. 
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    Eleven of tbe biochromophore compounds,2-(ω-biphenylyl) polymethylene-5-biphenylyl-oxazole-1 3,2-(ω-biphenylyl)polymethylene-5-biphenylyl-oxadiazolc-l,3,4 and their corresponding model compounds have been synthesized.Seven of the biochromophore compounds have not been reported in the literature.Their m.p. IR,1HNMR.MS, λmaxof UV spectra and fluorescence emission spectra have been determined. The structures of compounds 1.7 have been identified.
    Studies on Thermokinetics(Ⅴ)--Thermokinetic Method for the Second Order Reactions
    Wu Xiaoping, Qin Ziming, Deng yu, Cai Ruzen
    1987, 8(1):  55-59. 
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    On the theoretical basis of thcrmokinetics proposed in previous article, the method of dimensionless paramter for second order reactions are derived in thispaper.This method has been used to study the saponification of two csters in aqueous alcohol solvents. The rate constants of these reactions calculated with this method are in agreement with the values in literatures. And therefore, the fundamental equations of thermokinctic method for second order reactions are believed to be correct.
    Synthesis of Rare-Earth Monochloroacetate Hydrates and Measurement of Their Dehydration Enthalpies
    Wu Shurong, Xiong Weimiao
    1987, 8(1):  60-64. 
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    In our laboratory seven hydrated rare-earth monochloroacetates, Ln(CH2ClCOO)3·xH2O(x= 1.5, Ln = La,Ce,Pr,Sm,Eu; x=2,Ln = Nd,Gd) have been synthesized and characterized by elemental analysis, thermogravimetry and dehydration over P2O6The X-ray powder diffraction data of the salts have been obtained by X-ray measurements. The thermal dehydration processes studied by TG, DTG, DTAtechniques show that the salts lose crystallization water through a single-step to yield anhydrous salts. Their dehydration enthalpies were estimated by DSC, the determinated values of enthalpies were of the precision and accuracy of 2%.
    A Study on Indapamide and Its Synthesizing Intermediates by NMR
    Zhao Chengzhi, Xu Qinglun
    1987, 8(1):  65-69. 
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    Indapamide (Ⅰ) is a antihypcrtensive drug with high efficacy and long-time activity, which is recommended by many experts worked at international medicine circles. We have synthesized this compound and determined its 1HNMR spectrum. Also, 1H and 13CNMR spectra of intermediates (Ⅱ-Ⅶ), which are formed in the process of synthesis of compound (Ⅰ), are determined. The rotational isomerism of the compound (Ⅲ) was observed at the room temperature. Another analysis method on chemical shifts in ABXspin system was discussed.
    IRC Approch to Isomerization of Thioformaldehyde
    Li Xuekui, Li Zhesheng, Sun Chiachung, Zhao Chengda, Xia Xinfu
    1987, 8(1):  70-72. 
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    Isomerization (H2CS→HCSH) of . thioformaldchydc is studied by means ofintrinsic reaction coordinate (IRC) method. The thecrctical results of transitionstate and the normal coordinates are presented. The geometry optimization of the reactant, the transition state and the tracing of IRC have been performed by using the energy-gradient method with the split-valence 4-31G basis set. The results are obtained in agreement with the experimental data.
    Activity Coefficients of HCl in the System HCl-KCl-PrOH-H2O from 5 to 45℃
    Li Zijun, Yang Jiazhen, Liang Chunyu
    1987, 8(1):  73-75. 
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    This paper reports that emf of cellPt,H2(latm) |HCl(mA),KCl(mB),RrOH(x),H2O(1-x) | AgCl-Ag(A) have been made at 5-45℃ regions and x= 0.02,0.05,0.08 and 0.12, where x is molar fraction of PrOH in mixed solvents.The results show that HCl also obeys Harned' s Rule and logarithms of activity coefficients of HCl are a linear function for temperature.Relative patial molar enthalpy of HCl have been discussed.
    Study of the Infrared Absorption Spectra and the Photodecomposition of Solid Uranyl Formates
    Xu Baoyu, Gu Weixing, Chen Daming
    1987, 8(1):  76-78. 
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    Aseries of Solid uranyl formates ere prepared and their infrared absorption spectra were investigated. It was found that the anti-symmetric vibration frequencies of uranyl group,vα,for these compounds were in the range of 912-952 cm-1,and the vα absorption peaks were single-shaped for some uranyl formate double salts. According to above vαabsorption spectra,the decomposition of basic uranyl formate was also investigated by using TEA-CO2laser. The experimental results showed that the photodecomposition reaction could take place only under intense irradiation at the frequency resonant with the vα of uranyl group.
    Study on Coated-Carbon CdBr42-Ion Selective Electrode
    Cai Lizhen, Li Lanfu, Ren Yi
    1987, 8(1):  79-80. 
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    Acoated-carbon (PVCmembrane) CdBr42-ion selective electrode based on the trioctyldodecyl-tetrabromocadmiumate (Ⅱ) ion pair is described. The electrode exhibited Nernstian response for cadmium (Ⅱ) in 1M NaBr solution with a slope of 31±1mV decade over the concentration range 10-1-10-6Mat 25.5℃.Other performance parameters of the electrode and its application have also been reported.
    Studies on the Synthesis of α-Aminopyridine Resins and Capacity of Sorption and Desorption of These Resins for Au (Ⅲ)
    Wang Shouting, Chen Weizhu, He Biuglin
    1987, 8(1):  81-86. 
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    α-Aminopyridine ion exchange resins (APR) were synthesised by introducingα-aminopyridine into different polymer matrixes. The capacity of sorption and desorption for Au(Ⅲ) and the selectivity of these resins were studied. The effect of the structure of the polymer matrix on the resin properties was investigated.
    Synthesis, Structure and Behavior of Polymeric Drugs Covalently Linked 5-Fluorouracil
    Zhou Chaohua, Yang Fushun
    1987, 8(1):  87-92. 
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    Four scries of macromolocular drugs covalently. linked 5-fluorouracil(5-FU) are synthesized by the use of soluble starch and carboxylmcthylccllulose as carries, and two new 5-FUderivatives by the use of molecular sieve as catalyst. Their structure arc determined by R, 1HNMR and mass spectra. The changes for the nitrogen content of polymeric drugs with reactions and the influence of the Ncontent on their limiting viscosily arc studied. The hydrolysis delivery of 5-FUfrom starch and carboxymethyl-cellulose derivatives in various of buffer arc researched by moulding physiologicaly acid-alkali enviroment. In addition, antican-car activity (in vivo and in vitro) of some starch derivative has been prelimina-ryly observed.
    Studies on the Thermal Oxygen Stability of Xanthan Gum
    Wang Derun, Zhang Weidong, Zhao Dajian, Shang Baoxu, Chen Shenzhi
    1987, 8(1):  93-95. 
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    The thermal stability of xanthan gum have been studied by DTA, TG and Fourier IR. The results show that xanthan gum of China is decomposed at about 255℃, but that of U.S. is decomposed at about 250℃.
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