Table of Content

24 December 1988, Volume 4 Issue 4

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Articles

Studies on the Structure, Properties of Ferroaluminophosphate Molecular Sieve (FAPO-5) and Chemical State of Iron in the FAPO-5 Molecular Sieve

Han Shuyun, Yang Chuncai, Guo Ye, Wei Quan, Zheng Yingguang

1988, 4(4):  1-8. 

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The pure Ferroaluminophosphate molecular sieve(FAPO-5) was synthesized by hydrothermal crystallization. The crystal structure of FAPO-5 was studied via XRD, electron probe energy dispersion analysis, Mössbauer spectroscopy, EPR, XPS and IR, the parameters of unit cell and chemical composition of FAPO-5 were determined. The result has that the structure of FAPO-5 is AlPO₄-5 type and Fe²⁺ Fe³⁺ are incorporated into the framework of FAPO-5 molecular sieve. In addition, the chemical state of iron in FAPO-5 molecular sieve were studied and the adsorption properties, surface acidity and thermal stability were also investigated.

Preparation of Hexa-and Decatungstates Through Oxidation of Tungsten Carbide with Hydrogen Peroxide

Gu Yidong(Yih-Tong Ku), Shao Cuiqi, Chen Mingqin

1988, 4(4):  9-15. 

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The reaction of tungsten carbide with hydrogen peroxide, followed by addition of tetra n-butgl ammonium chloride, gives principally colorless hexatungstate and yellow decatungstate at room temperature and 60℃. The compound, heteropoly tungstate with carbon as the central atom, as suggested by K. Tetsuichi, has not been obtained.

Simultaneous Spectrophotometric Determination of Cadmium, Zinc and Copper with Kalman Filter

Zhang Zhengqi, Liu Yimin, Yu Ruqin

1988, 4(4):  16-23. 

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The compound 2-QADNm can form red complexes with caamium(II), zinc(II) and copper(II). The simultaneous determination of cadmium, zinc and copper with Kalman Filter is described in this paper, the proposed method was applied to a two-component system for determining cadmium and copper,and a three-component system for determining cadmium, zinc and copper.

Studies on Single-electron Oxidation of N-Alkyl-p-Phenylenediamines and Benzidines in Aqueous Acetonitrile by Cyclovoltammetry and ESR Spectroscopy

Zhang Fa, Gao Zhongli, Liu Youcheng, Chen Wei

1988, 4(4):  24-31. 

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It is demonstrated by cyclovoltammetry and ESR spectroscopy that N,N,N,'N,'-tetramethyl; tetraethgl, tetra-n-propyl, tetra-n-butyl-p-phenylenediamine and tetraethyl, tetra-n-propyl-p-benzidine undergo deprotonat ion and two consecutive single electron transfer step CE reaction at electrode in aqueous acetonitrile with the corresponding radical cations as the intermediate. The bivalent cations produced at the electrode react not only with hydroxyl anion in the medium to give quinone but also with the N-alkyl-p-phenylene-diamines or benzidines to produce the corresponding radical cations.

Studies on the Syntheses of the Side Chains of Brassinolide and Dolicholide

Mao Jianmin, Hou Zijie, Liu Xingping, Li Yulin

1988, 4(4):  32-38. 

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(4R,5S)-2,2-Dimethyl-4-(1',2'-dimethylpropyl)-5-(1'-bromoethyl)--1,3-dioxolane(15) with the side chain of brassinolide and (4R, 5S)--2, 2-dimethyl-4-(l'-methylene-2'-methylpropyl)-5-(1'-bromoethyl) 1,3-dioxolane(14) with the side chain of dolicholide were first synthesized through 11 and 10 stepes from D-mannitol respectively. All of the intermediates 7～13 were first synthesized too.

Studies on the Chemical Constituents of Oxytropis Glabra DC (I)

Sun Rongqi, Jia Zongjian, Zhu Ziqing(Chu Tsetsin), Chen Nenyu, Zhao Fanzhi

1988, 4(4):  39-43. 

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Two new triterpenoid sapon.ins 1 and 2 were isolated from the crude saponin extract of Oxytropis glabra DC by Si gel chromato-grapny . Saponins 1 and 2 were determined to be 3-0-1 β-D-glucopyranosy 1 (1-2)- β -D-glucuronopyranosyl azukisapogenol methyl ester and 3-O-[β-D-glucopyranosyl(1 - 2 ) - β -D-glucuronopyranosyl] azukisapogenol amide, respectively by spectral analysis and chemical methods.

Synthesis and Spectra of Bichromophore Compounds Containing Oxazole or Oxadiazole Ring

Zhou Yimin, Wang Shenxiu, Kao Chenheng

1988, 4(4):  44-52. 

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Fifteen of the bichromophore compounds containing oxazole or oxidation ring have been synthesized. Their structures have been identified by IR, ¹H NMR spectra and elemental analysis. The UV spectra, fluorescence spectra and the laser conversion efficiencies have been determined . The results of determination show that the absorption and emission spectra Pf the bichromophore compounds are different from those of the corresponding single chromophore compounds.

Study on the Biomimetic Oxidation Catalyzed by the Model Compound of Cytochrome P-450(VI)——The Influence of Substituent x in T(x-p)PMn(Ⅲ)Cl on the Hydroxylation of Alkane

Zhu Shenjie, Gu Chen

1988, 4(4):  53-60. 

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The influence of monosubstitution at phonyl rings in a series of T(x-P) PMn (Ⅲ)Cl (x = o, m, p-CH₃, CH₃O, Cl, Br, I, NO₂, o-NH₂, p-(CH₃)₃C) on the biomimetic catalytic hydroxylation and chlorizaiton of cyclohexane with PhIO was studied. The yields of cyclohexanol and chlorocyclohexane increased with the electron-withdrawing ability of the substituent in this manganese complex. The fair linear correlations between the yields of cyclohexanol and para or ortho substituent constant are presented as:logY_x/Y_H = 0.31σ_p+0.03, logy_x/Y_CH3 = 0.61σ^*0.07E_s+0.05, But there are no linear correlations between the yields of chloro-cyclohexane and either para, ortho or meta substituent constants.

The Crystal and Electronic Structure of A Reticular Type Mo-Fe-S Cluster Compound [Et₄N]₄[Mo₂Fe₄S₉（SCH₂CH₂S）₂]

Fan Yuguo, Zhang Zhigui, Guo Chunxiao

1988, 4(4):  61-70. 

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The single crystal of [Et₄N]₄ [MO₂Fe₄S₉(SCH₂CH₂S)₂] was obtainedby reaction of (NH₄)₂HoS₄, FeCl₃, HSCH₂CH₂SH and Et₄ NBr in CH₃CN and MeOH-MeONa. Cluster compound [Et₄N]₄[Mo₂Fe₄S₉(SCH₂CH₂S)₂] crystal -Lized in the monoclinic space group C₂/c with unit cell parameters:a = 17. 672(2)Å, b = 33. 851(4)Å, c = l3. 900(3)Å, β=135.11(4)°, V=5868.8 (3.9)ų and Z = 4. On the basis of 3514 unique data (I>2σ(I)) the structure was refined to R = 0.0575. The anion [Mo₂Fe₄S₉(SCH₂CH₂S)₂]^4- of the cluster compound includes doubly bridging (μ₂-S), triply bridging (μ₃-S) and quadruply bridging (μ₄ -S) . The structrue analysis gives a rule with bond lengths decreasing in the order of Fe-(μ₄-S)> Fe-(μ₃-s)> Fe-(μ₂ -s) and EHMO calculation gives the other rule with bond order increasing in the order of Fe-(μ₄-S)< Fe-(μ₃-S)<Fe-(μ₂-S). The experimental and theoretical results are in good agreement. According to the nearby energy level arrangement of front orbit the author considers that it has six unpaired electrons and spin of 3. The measurement of magnetic moment proved that the result of EHMO calculation is correct On the basis of summarization on structural parameters of relative Mo-Fe-S cluster compound and the data of Mo(Fe) valence state the authors suggest that the terminal bond of Mo-St is a more effective monitor of oxidation states and the Mo and Fe atoms in the title cluster compound have oxidation states of +5 and +2 respectively. The cluster anion [Mo₂Fe₄S₉(SCH₂CH₂S)₂]^4- isarranged in a structure of idealized C₂ symmetry in which the C₂ axis contains μ₄ -S (7) . There are three types in cation Et₄N⁺: (1) general position, (2) special position, C₂ axis passes through N atom,(3) special position, C₂ axis passes through a terminal C. The local disorder of Et₂N⁺ in special position appears as result of requirement of C₂ axis.

Kinetics of Catalytic Hydrolysis of Potato Starch by Immobilized β-Amylase

Li Xuyuan, Wang Shouyu, Liu Shengzhong, Hao Xiangying, Meng Yimin

1988, 4(4):  71-76. 

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The enzyme activity of immobilized β-amylase carried on active carbon and the reaction kinetics for hydrolysis of potatostarch catalyzed by the enzyme have been investigated. A kinetics model based on the overall reaction has been suggested and a reaction coefficient as a new parameter introduced. All of the kinetics parameters involved in the model, including the reaction coefficient, reaction order rate constant as well as the maximum reaction rate etc. at different temperatures have been obtained by using the modified Quasi-Newton optimization technique.

Li⁺,Na⁺//Cl^-,B₄O₇^2-—H₂O Reciprocal Quaternary System Solubility Phase Diagrams

Ma Peichao, Chen Peiheng

1988, 4(4):  77-83. 

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The solubilities, refraction indices and densities of saturated solution of Li⁺, Na⁺// Cl^-,B₄O₇^2- -H₂O reciprocal quaternary system at 0℃, 25℃ and 50℃ were determined by using isotherm method. Using total concentration of all the salts in solution as concentration coordinate(ordinate) the isothermal stereogram of solubility of the system was drawn. The results showed that the stable salt-pair of the system is Na₂Cl₂-Li₂B₄O₇ and that there are two isothermal invariant points, eutonic ponit E and inversion point P corresponding to the eqilbria: solution (E)(这里有图片19880411-77-1.GIF)LiCl·H₂O (at 25, 50℃) or LiCl·2H₂O (at 0℃) + NaCl + Li₂B₄O₇ · 3H₂O and solution (P) + Na₂-B₄O₇·1OH₂O(这里有图片19880411-77-1.GIF)NaCl + Li₂B₄O₇·3H₂O and the crystallization fields ofborates are much larger than those of chlorides.

Studies on Inorganic Ion Exchanger Containing Phosphorus(IX)——Kinetics of Ion Exchange Reaction for Alkaline Earths on SVPP

Xia Jinlan, Liu Jinchun, Liu Liangbin, Cheng Jieke

1988, 4(4):  84-89. 

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A shell reaction mechanism and its mathematic model were used to inquire into the kinetics of ion exchange reaction between alkaline earth metal ions and H^- form of micro-crystalline SVPP.The activation energy ( E_a), entropy of activation (ΔS^*) and self-diffusion coefficient ( D_o ) of alkaline earths were calculated bysolving the Nernst-Planck equations on a IBM-PC computer. The linear relations between the bare ionic radii of alkaline earths r_o and E_a, ΔS^*or lgD_o have been obtained.

Selective Oxidation of Secondary Alcohols in the Presence of Primary Alcohols by an Oxoammonium Salt

Liu Youcheng, Liu Zhongli, Guo Honnxun

1988, 4(4):  90-94. 

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