Table of Content

24 June 1986, Volume 2 Issue 1

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Articles

STUDIES ON THE COMPETITION FOR CADMIUM ION BETWEEN CHELATING AGENTS AND BOVINE SERUM ALBUMIN

Li Rongchang, Chen Baowei, Wang Kui, Wu Yonghui, Wang Xiangyun

1986, 2(1):  1-7. 

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Eleven chelating agents were studied for their capabilities to mobilize the cadmium bound tp bovine serum albumin(BSA).The parameter F,which is defined as the ratio between the percentages of cadmium bound to BSAin the presence and absence of chelating agents,can be used as the criterion to evaluate the mobilizing capability of chelating agent.The Fvalues determined experimentally lead to a mobilizing capability order:DTPA>EDTA>EGTA>NTA>TR1EN>PEN>CYS>HIS>SAThe polyaminopolycarboxylate type chelators mobilize cadmium effectively.Alinear relationship was found between₁gFand lg k'CdL (conditional stability constant of the cadmium chelate).

STUDIES ON ORGANO-MOLYBDENUM AND TUNGSTEN COMPOUNDS(Ⅲ)——CATALYTIC POLYMERIZATION OF ACETYLENE BY M-O-C BOND-CONTAINING COMPLEXES OF Mo AND W

Liu Dehai Ye Dakeng, Liu Daoyu

1986, 2(1):  8-12. 

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Catalytic polymerization of acetylene in the presence of n⁵-C₅H₅-M-(CO)₃ R (M=Mo,W;R=CH₃-,C₂H₅-) has been studied.The results show that these complexes possess catalytic activities for the polymerization and copolymerization of monosubstituted acetylene.The catalytic mechanism has been preliminarily discussed.It is suggested that the active species be metal-car-bene.In our previous publications we reported the synthesis of some new Fischer’s molybdenum and tungsten-carbene complexes and catalytic activity for alkyne polymerization.The results show that the activity of Fischer’s molybdenum-carbene is higher than that of tungsten.The catalytic polymerization of alkyne by M-σ-c bond-containing complexes of molybdenum and tungsten has not been reported yet in literature.Therefore,four M-σ-Cbondontaining complexes of molybdenum and tungsten were synthesized by using the method reported in the literature,and catalyst polymerization of alkyne by these complexes was examined.

ANALYSIS OF VOLATILE CONSTITUENTS OF CHINESE MEDICINAL HERBS BY FLASH DISTILLATION/CAPILLARY GAS CHROMATOGRAPHY/MASS SPECTROMETRY

Chen Yaozu, Li Zhaolin, Xue Dunyuan, Han Hui

1986, 2(1):  13-18. 

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In present work,the volatile constituents of Curcuma longa L.,A.lancea (Thunb.) DC.,Foeniculum vulgare Mill,and Cinnamomun cassia Presl.have been analyzed by flash distillation/capillary gas chro-matography/mass spectrometry.The results are consistent with those obtained by conventional steam distillation extraction method.The optimum condition of flash distillation has been studied.The experimental results showed that this new technique proved to be a simple,rapid and efficient tool for microanalysis of volatile constituents of Chinese medicinal herbs.

THE MASS SPECTRA OF HKTEROCYCLIC CONJUGATED COMPOUND AND ITS QUANTUM CHEMICAL CALCULATIONS

Fang yaoren, Lai Zhugen, Liang Desheng, Lu Fengcai

1986, 2(1):  19-24. 

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Amechanism of cleft-rate-determining-step of furfurol,furylacrylic acid,dimethylfuran,thiophene-2-aldehyde,and pyrrole-2-aldehyde is.proposed,and various quantum parameters of molecular ions of these compounds and their fragments are calculated by using CNDO/2 method.The peak-height of mass spectra is quantitatively interpreted.This method could be extended to heterocyclic conjugated compounds.

’STEREOSELECTIVE SYNTHESIS OF TRISIJBSTITUTED ALKENES VIA,TITANOCENOCYCLES

Liu Yiyin, Chen Meiwen, Li Yan, Wang Jitao

1986, 2(1):  25-32. 

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By previously reported modified Masai-Rausch method of synthesizing titanocenocycles,followed by acid hydrolysis,trisubstituted al-kenes were synthesized,yields obtained are higher than that reported in literatures.Starting from unsymmetrical alkyne substrates,twelve different types of substituted alkenes were synthesized,among which only two were found single component,others were of mixed isomers.Beside conventional analytical methods,the NMRspectral analysis of titanocenoheterocycle intermediates and the products were used to identify the isomeric structures as well as their relative contents.

THE SYNTHESES OF DERIVATIVES OF CYCLIC NUCLEOTIDE

Zhang Lihe, Ma Lingtai, Xu Cheng, Dong Lingjiao, Hang Qi, Wang xu

1986, 2(1):  33-40. 

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By using triphenyl phosphine/carbon tetrachloride as a condensing reagent,2’-tosyl c-AMPreacted with RR-NHto give nucleoside 3’,5’-cyolic phosphoramidates in 28-55% yield.Esterification of 2’-tosyl c-AMPcan be carried out in acetonitrile with alkyl toluenesulf-onate.Detosylation can be completed by using sodium napnthalide at-78℃ in DME.The stereoisomers of these compounds have been separated and the structures were identified by 1H NMR.31P NMRand MS.

PHOSPBORYLATION REACTIONS OF BENZOTHIAZOLONE

Chen Kajian, Zhang Jinglin

1986, 2(1):  41-48. 

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This paper reports the reactions of benzothiazolone with phosphites,tris-(dialkylamino)-phosphines and bis-(dialkylamino)-phen-ylphosphines.Benzothiazolone could not react with various phosphites,but it gave N-phosphorylated products when reacted with phosphorus amides.The restricted rotation about P桸 bond at room temperature was observed and discussed.

DEVELOPMENT OF DOUBLE-BARRELED CALCIUM ION-SELECTIVE MICROELECTRODE

Zhuang Yunlong, Zhou Jianping, Qi Deyao

1986, 2(1):  49-54. 

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Anew PVCmatrix membrane double-barreled calcium ion-selective microelectrode based on liquid ion exchanger has been designed and constructed.The tip diameter of about 2.5μm as well as lower selectivity coefficients for K⁺,Na⁺ and Mg²⁺ are adequate for in-tracellular measurements of Ca⁺ activities.The inner wall of the selective channel was made to be hydrophobic by treatment withalkyl-alcohols.By means of this microelectrode some physiologicalphenomena related to Ca²⁺ activities have been studied,and Caconcentrations in clinical microsamples have also been determined.

STUDIES ON THE DISSOCIATION OF THE RARE-EARTH CHROMOGENIC REAGENT CHLOROPHOSPHONAZO-mA

Zhao Hong, Zhu Chuanzheng, Zhou Weiliang, Pan Jiaomai

1986, 2(1):  55-64. 

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Chlorophosphonazo-mA [2-(4-Chloro-2-phosphonobenzenenazo)-7-(3-ac-etylbenzenenazo)-1,8-dihydroxynaphthalene-3,6-disulfonic acid] is a derivative of unsyr.metrical bisazo chromotropic acid,with the following structure In 1979,it was first reported that the title compound could be used in the spectro determination of the total amount of micro rare-earths existing in spherical graphite cast iron and weak alloy steel and direct spectro determination of the total amount of the rare-earths and the fractional amount of the light and heavy rare-earths when used together with chlophosphonazo-mN It is a rather ideal chromogenic reagent to determine the total amount of the rare-earths.It was also discovered in later work to be usefulin the spectro determination of the elements uranium(VI)and calciumetc. In order to make a further study for the thermodynamic properties and kinetic characteristics of the reagent when complexing with the rare-earths we have first investigated the ionization of the chlorophosphonazo-mAin solution.This paper reports the results of determining the successive ionization constants and the thermodynamic parameters of each step of chlorophosphonazo-mAby pHpotentiometric and spectrophotometric methods.

SPECTROPHOTOMETRIC STUDY OF BIMETALLIC TERNARY COMPLEX OF LANTHANUM——COPPER WITH ALIZARIN FLUORINE BLUE

He Xiwen, Li Hong, Shi Huiming

1986, 2(1):  65-75. 

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The bimetallic ternary complex formation in the aqueous solution of La³⁺ and Cu²⁺ with alizarin fluorine blue (AFB) was studied by spectrophotometry.The ternary complex LaCu₃(AFB)₃ has maximum light absorption at 550nm.The colour reaction selectivity is fairly good and the method can be applied to the direct photometric determination of copper in lanthanum or some pure metals.Anew mathematical approach to the treatment of spectrophotometric data for differentiation between mononuclear and polynuclear in solution is presented.The improvable fixed logarithm method is for complexes of the type M_mB_n(m=n) or M_mB_n(m=n).We report that La(Ⅲ) combines with AFBat pH 4.5 to form a single complex,withm=n=2,La₂(AFB)₂.

OPTIMAL SCHEME FOR SEQUENTIAL COMPUTATIONS OF F_m(z) INTEGRALS IN AB INITIO CALCULATIONS----COMBINATORY USE OF UPWARD AND DOWNWARD RECURSIONS

Liao Muzhen, Wu Guoshi, Chen Kaixian, Liu Honglin, Chen Nianyi

1986, 2(1):  76-84. 

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The quantitative rules of the transfer and variation of errors,when the Gaussian integral functions F_m(z) are evaluated sequentially by recurring,have been expounded.The traditional viewpoint to negate the applicability and reliability of upward recursive formula in principle is amended.An optimal scheme of upward-and downward-joint recursions has been developed for the sequential F_m(z) computations.No additional accuracy is needed with the fundamental term of recursion because the absolute error of F_m(z) always decreases with the recursive approach.The scheme can be employed in modifying any of existent subprograms for F_m(z) computations.In the case of p-d-f-and g-type Gaussians,combining this method with Schaad’s formulas can reduce,at least,the additive operations by a factor 40%;the multiplicative and exponential operations by a factor 60%.

NATURE OF THE A AND THE F MATRIX IN THE CALCULATION OF FORCE CONSTANTS OF MOLECULAR VIBRATION

Van Guosen, Sun Zemin, Xiao Shenxiu, Zhou Xuefeng

1986, 2(1):  85-92. 

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In this paper,calculations of force constants of molecular vibrations are carried out by using Wilson GFmatrix method.In the determination of force constants from frequencies and factorization of Gmatrix,an ordering relationship of Amatrix(may be n dimensional) relative to Lmatrix was found according to the ordering of symmetry coordinates.With the help of inverse unitary transformation,a general method to calculate Ft from constants Fs was established.The additivity of Fr depending on the symmetry block was determined to be true.All the force constants in non-planar and planar of urea,thiourea and sclenouroa molecules were calculated by using the general va-leine force field.The calculated values of frequencies were com-pairec with other data given in the literature,and it was shown that the present calculation is in good agreement with the experimental

SUIDIES ON SOME PROPERTIES AND CATALYSIS OF RARE EARTH HETEROPOLY ACIDS

Wu Zhiyun, Zhao Zhongqing, Jiang Min, Li Kai, Zhang Qiang

1986, 2(1):  93-96. 

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Though potassium salts of rare earth substituted silicotungsticacids were synthesized early in 1971 by R.D.Peacock etc.,sofar the reports about the application of the corresponding acidshave not been found.We prepared fourteen rare earth substitutedsilicotungstic acids and determined their thermal stability,IRabsorption Spectra and x-ray diffraction spectra.Furthermore,thecatalytic activities of the fourteen heteropoly acids in acid cata-lytic reaction were investigated.Our experimental results demonstrated rare earth substituted silico-tungstic acids have very high catalytic activity in the reaction of

EFFECT OF DISPERSED PHASE PARTICLES ON ELECTRICAL CONDUCTION OF PEO-NaSCN

He Yuankang, Chen Zhusheng, Zhang ZhiyiWang Chaoying, Chen Liquan

1986, 2(1):  97-101. 

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Fast ionic conductors are one kind of solid state material with ionic conductivity as high as that of melten salts or liquid electrolytes.Ionic conductivity is one of the important parameters for characterizing a fast ionic conductor.For a long time materialists and chemists have made great efforts in search of new fast ionic conductors with high ionic conductivity.In view of structure,they have synthesised silver and copper fast ionic conductors with so called open structures.But it is not so successful for searching more applicable alkaline fast ionic conductors.Since polymer has flexibility for making thin film,it concentrates attention on the polymer-alkaline salt complex.Fenton et al.have first reported poly(ethylene oxide) (PEO)-alkaline salt complex.Later on Armard et al.have investigated the electrical property of PEO-NaSCN.