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    24 November 1986, Volume 7 Issue 11
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    Articles
    Synergic Extraction of Rare Earth Elements With Phenanthroline and Hydroxy-Isobutyric Acid, Salicyl Acid
    Han Dongmei, Ni Zhaoai
    1986, 7(11):  959-964. 
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    The extraction of all rare earth elements(except Pm)from thiocyanatc solution with mixtures of phenanthroline(Phcn)and hydroxy-isobutyric acid(HHIBA),salicyl acid(Hsal)in chloroform has been investigated.The results of experiments show that there is obvious 'synergic effects' either in the system of-RE(w)3+HHlIBA(0)-Phen(0)-SCN-(w)or in the system of RE(w)3+-Hsal(0)-Phen(0)SCN(w)and there exists obvious 'tetrad effects' in the two synergic system.
    Studies on the Synthesis, Structure and Properties of Zeolite ZSM-5 with Gallium Contained
    Wu Yuyao, Zhou Eengqi, Liu Xinsheng, Zhao Daqing, Duan Binsheng
    1986, 7(11):  965-968. 
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    Ga containing ZSM-5 type zeolite with a ratio of SiO2/Ga2O3 being60-38 has been synthesized from water glass,gallium trichloride,1,6-hexanediamine HXDAand water at 150-170℃ without addition of crystal seeds and directing agent.The X-ray diffraction pattern showed that Ga-ZSM-5 type zeolite similar to zeolite ZSM-5.The cell parameters.a=20.2lÅ=20.04Å,c=13.47Å,were obtained by step scanning technique.An electron probe analysis was conducted,which shows gallium entered the framework of the zeolite.The adsorption proper-lies,acidity,thermal stability and IRspectra were also determined.
    Studies on the Hydrolytic polymerization of Ghromium(Ⅲ) Ion(Ⅷ)-The Transition Stage in the Presence of Fumaric Acid
    Luo Qinhui, Shen Mengchang, Ding Yi, Tu Qinyun
    1986, 7(11):  969-974. 
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    Hydrolytic polymerization of chromium(Ⅲ)inM Cr(NO3)3 aqueous solution in presence of fumaric acid of four different concentrations(0.0035,0.005,0.0075,0.01M)was studied.The results show that the state of chromium(Ⅲ)is guite complicated,and besides the species([Cr2(OH)A]3+,[Cr2(OH)A2]+,[Cr(OH)A])which exist in high and low concentration regions,new species([Cr2(OH)2A]2+has also been found,so this region may be regarded as transition stage,The species in the transition stage would transform one to another as the concentration changes.It shows some analogy with the results presented previously.Such phenomenon is rarely observed in hydrolytic reaction of other metal ions.Hydrolysis constants are calculated by program LEMITand values of identical species obtained in the different concentration regions of fumaric acid are in good agreement with each other and agree with those reported in the previous papers.
    Partial Fusibility Diagrams of NdCl3-KCl NaCl NaF and NdCl3 KClNaCl CaF2 Systems
    Li Ping, Pang Wenqin
    1986, 7(11):  975-977. 
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    In order to prevent moisture regain and hydrolysis of specimen,a method of directly chlorinating the rare earth oxide is recommended for thermal analysis of the systems containing rare earth chlorides.Using the method,partial fusibility diagrams of NdCl3-KCl·NaCl-NaFand NdCl3-KCl·NaCl-CaF2 systems arc constructed.
    The Application of Non-Zero Isosbestic Point in the Double-Wavelengtn Spectrophotometry
    Li Jinhe, Shi Huiming, Wang Xiaofeng
    1986, 7(11):  978-981. 
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    In this paper the photometric behavior of Al(Fe)-CAB,Al(Fe)-CASin the presence of mixed surfactants and the feasibility of non-zero isosbestic point in the double-wavelength spectrophotometry have been studied.The present method is successfully applied to the simultaneous determination of Al and Fe.
    Studies on Polarographic Behavior of2,7-TADN (Ⅱ)-Polarographic Adsorptive Complex Wave of Copper -2,7-TADN-Ethylenediamine
    Zhang Zhengqi, Yang Xia, Yu Jin, Yu Ruqin
    1986, 7(11):  982-985. 
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    In a sodium hydroxide solution of pH12 containing ethylenediamine(en)and 1-(2-Thiazoiylazo)-2,7-Naphthalenediol(2,7-TADN)a sensitive adsorptive complex wave of Cu(2,7-TADN)(en)was observed by using single-sweep polarography.The peak potential is-0.86V,the peak hights being linearly proportional to copper concentration over a range of 2.0×10-8 to 5.0×10-6M.The determination limit is 1.0×10-8M.This method has been applied to determine trace amount of copper in ores and pure tin.In a sodium hydroxide solution of pH12 containing ethylenediamine(en)and 1-(2-Thiazoiylazo)-2,7-Naphthalenediol(2,7-TADN)a sensitive adsorptive complex wave of Cu(2,7-TADN)(en)was observed by using single-sweep polarography.The peak potential is-0.86V,the peak hights being linearly proportional to copper concentration over a range of 2.0×10-8 to 5.0×10-6M.The determination limit is 1.0×10-8M.This method has been applied to determine trace amount of copper in ores and pure tin.
    The Extraction Spectrophotometric Determination of Palladium with2-Mercapto-β-Naphthothiazole (MNT)
    Fan Shaoying, Wang Jianhua, Zhao Mingren, Wang Huiqin, Yang Wenzhong
    1986, 7(11):  986-988. 
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    Amethod for the solvent extraetion-spectrophotometric determination of palladium with 2-mercapto-β-naphthothiazole（MNT）has been studied.The complex in acidic solutions,palladium（Ⅱ）reacts with MNTto form a complex which can be extracted into organic solvent phase,benzene and so on.The absorption maximum of the palladium complex in benzene was found at 440nm with apparent molar absorption coefficient of l.01×104 mol-1cm-1.The complex can be quantitatively extracted with benzene from the range of pH0～3,but not from alkaline solution.Beer's law is confirmed over the range of 0～100μg of palladium in10 ml of benzene.
    New Techniques in Electrometric Titration
    Xu Weijian, Gao Hong
    1986, 7(11):  989-991. 
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    Five new techniques in electrometric titration are described.They are:Ⅰ Oscillopolarographic titration at 1 micro and 1 macro Pt-electrodes.Ⅱ.Oscillopolarographic titration at 3 electrodes.Ⅲ.Oscillo-potentiometric titration at 3 electrodes.Ⅳ.Oscillo-potentiometric titration at 1 micro and 1 macro Pt-electrodes.V.A.C.Oscillo-potentiomctric titration at 2 macro Pt electrodes.The methods Ⅰ and Ⅱ use the abrupt change of oscillopolarogram to indicate end-point but do not require the oscillopolarograms to have a sensitive incision.The others do not use any oscillopolarogram but use the abrupt potential change between electrodes.Five new techniques in electrometric titration are described.They are:Ⅰ Oscillopolarographic titration at 1 micro and 1 macro Pt-electrodes.Ⅱ.Oscillopolarographic titration at 3 electrodes.Ⅲ.Oscillo-potentiometric titration at 3 electrodes.Ⅳ.Oscillo-potentiometric titration at 1 micro and 1 macro Pt-electrodes.V.A.C.Oscillo-potentiomctric titration at 2 macro Pt electrodes.The methods Ⅰ and Ⅱ use the abrupt change of oscillopolarogram to indicate end-point but do not require the oscillopolarograms to have a sensitive incision.The others do not use any oscillopolarogram but use the abrupt potential change between electrodes.
    Computer Simulation of Modified Simplex Method and Its Application in Ghemiluminescence Analysis
    Chen Guonan, Zhang Fan
    1986, 7(11):  992-994. 
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    The basic principle of modified simplex method(MSM)is elaborated.The optimization process of MSMis simulated by computer on the basis of the mathematical principle of MSM.The simulation program written in BASICis successfully operated on APPLE Ⅱ(FO-3)microcomputer.On the basis of above researches,it has been used in selection of the optimum reaction condition of the o-phenanthroline-H2O-CTMAB-Cu(Ⅱ)chemiluminescence system,and good results are obtained.
    Research on 2,5-Disufestituted Oxazoles(Ⅵ)-Solvent Effects on Spectra of 2-p-biphenyl-5-Phenyl Oxazoie and Some of Its5-p-Substituted Phenyl Derivatives
    Zhou Yimin, Yu Peifeng, Gao Zhenheng
    1986, 7(11):  995-1000. 
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    The UVabsorption spectra and fluorescence emission spectra of 2-biphenyl-5-phenyl oxazole and thirteen 5-substituted phenyl derivatives in 3 solvents have been measured.Abrief discussion on the relation between the substituent effects and spectra of the compounds is given.The solvent effect on absorption spectra and emission flurescence Spectra of 2-biphenyl-5-(p-ethyl)phenyl Oxazole in 19 solvents has been studied.
    The Synthesis of N-(α,β-Dihalo-4-Chlorocinnamyl)-secbutylamines
    Peng Shiqi, Liu Weiqin, Chen Suming, Qian Jinzhi
    1986, 7(11):  1001-1004. 
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    Tn this paper the synthesis of N-(α,β-dihalo-4-chlorocinnamyl)-secbutyl-amines was reported,the effect of reaction conditions on the reltaed proportions of Zand Eisomers in the products was discussed.The geometric configurations of these isomers were assigned based on NMR.
    Synthesis of Isoharringtonine Analogues-Cephalotaxine Methyl Tartrate
    Nie Xinyong, Li Shaobai, Li Yulin, Pan Xinfu
    1986, 7(11):  1005-1007. 
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    The(2R,3R)or(2S,3S)-Cephalotaxinc methyl tartrate acetonide Ⅳ or Ⅴ was prepared by the monocstcr exchange reaction of(2R,3R)or(2S,3S)-dimethyl tartrate acetonidc Ⅰ or Ⅱ with cephalotaxine Ⅲ under the catalysis of CH3ONa Compounds Ⅳ andⅤ were hydrolyzed by F3CCO2H-H2O(96:4)to give(2R,3R)and(2S,3S)-cephalotaxine methyl tartrate Ⅵ and Ⅶ,The ester exchange reaction may be employed in the preparation of the other analogues.
    Studies on C-Glycosides(Ⅲ)-The Reactions Between α-O-Tetraacetyl-D-Glucopyranosyl Chloride and Lithium Diarylcuprate
    Cai Mengshen, Dong Lingjiao, Wang Shaonong, Cheng Tieming
    1986, 7(11):  1008-1010. 
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    The preparation of lithium diarylcuprate and the reactions between lithium diarylcupratc and α-O-tctraacetyl-D-glucopyranosyl chloride were reported,1-β-Aryl-O-tetraacetyl-D-glucopyranosc,2-hydroxy-2,3,4,6-O-tetraacctyl-D-glucal from elimination reaction of acyl glucopyranosyl chloride,and a small amount of phenol,probably from the addition of water to benzyne were isolated from the reaction mixture by column chromatography.
    The TPD Study of CO2 From the Cu/ZnO/Al2O3 Catalyst for the Low Temperature Shift Reaction
    Duan Xue, Wang Qi
    1986, 7(11):  1011-1015. 
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    The desorption kinetics of CO2 from the Cu/ZnO/Al2 O3 catalyst for the low temperature shift reaction is studied by temperature programmed desorption(TPD).The Tf method of analyzing the complex TPDspectra is put forward and a count problem about the surface coverage θ in the complex TPDspectra is solved.The detailed analysis of the complex TPDspectra,with the method of T1 and desorption rate isotherms,gives the desorption kinetic parameters and determines the desorption rate equation.It is represented that the effective surface of the catalyst about CO2 is not an ideal surface.And it is also found that the desorption of CO2 from the catalyst is followed a first order process.The Arrhenius graph,lastly,is discussed.
    A Study of Surface Acid on Mimic Silica-Alumina Catalyst (Ⅱ)-The Basic states of Bronsted Acid and the Influence of Silicon-Aluminium Ratio on Bronsted Acdity
    Feng Jikang, Li Zhiru, Li Song, Zhang Wuyang
    1986, 7(11):  1016-1019. 
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    By applying EHMOmethod,a series of mimic calculations have been performed for the surface acid of Silica-Alumina catalyst,the basic states of Bronsted acid and the influence of Silica-Alumina ratio on Bronsted acidity have been studied.The calculations from different states of Bronsted acid show that the content of Aluminium in catalyst have a great influence upon the Dronsted acidity,and the forming of Al-O-Al structure is the essential reason for marked decrease of Bronsted acid strength.The results from theoretical calculations are in accordance with the experimental results of measurements of Bronsted acid.
    Study of Reaction Mechanism for Dehydrogenation of Ethylbenzene Over Iron-Oxide Catalysts(Ⅰ)-In-situ FT-IR spectra of Ethylbenzene Adspecies and Kinetic isotope Effects of the Dehydrogenation Reaction
    Chen Jianping, He Danyun, Cao Shoujin
    1986, 7(11):  1020-1025. 
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    The IRspectra of adspecies of ethylbenzene and ethylbenzene-d10 were observed at the room temp and reaction temp,respectively.The relative rates of dehydrogenation of several kinds of deuterium labelled ethylbenzene have been determined under the same reaction conditions.Apossible mechanistic pathway for the dehydrogenation of ethylbenzene may then be proposed as following.First,the ethylbenzene molecule is adsorbed on the iron oxide catalyst surface,the α-His abstracted by lattice oxygen of the catalyst to form a surface-OH,and a pseudo π-allyl intermediate of the ethylbenzene residual,which may be coverted to a pseudo σ-allyl intermediate The β-Hmay then be ruptured to form styrene molecule and a Fe-Hbond on a neighbouring Fe+2(+3)in the rate determining step.
    Theoretical Studies of the Electronic Structure and Molecular Vibration on Interstellar Cyanopolylacetylenes
    Yu Jianguo, Zheng Shijun, Tang Dinghua
    1986, 7(11):  1026-1030. 
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    The interstallar cyahopolyacetylenc(HC2nCN,n=0,1...,5)have been studied theoretically by means of MINDO/3 method.The linear relationships between HOMO,LUMOand total electronic energies ETwith n in cyanopolyacetylenes are found.On the linear relationships of these frontier orbitals,the larger the n,the higher the HOMOs' and the lower the LUMOs' in cyanopolyacetylenes.In consequence,the system is more unstable.On the calculated vibrational frequencies and the analysis of the mode of vibration,the existence of some characteristic vibrations such as H-Cstretch vibration about 3820 cm-1 and H-C-Cbent vibration about 800 cm-1 is predicted for cyanopolyacetylenes except HCN.
    Crystal and Molecular Structure of C5H5FeC6H4SO2N （C2H4CN）CH2C6H5
    Xin Min, Han Yuding, Liu Qiwang, Hu Yucai, Huang Jinsun
    1986, 7(11):  1031-1034. 
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    The crystal structure of C5H5FeC5H4SO2N(C2H4CN)CH2C6H5 was determined by X-ray analysis The crystal is monoclinic,belonging to space group P21/n with unit cell dimensions.a=8.750(1),b=12.876(5),c=16.744(2)Å β=94.75(1),V=1880.0Å3,Z=4,Dc=1.442g/cm3.The intensities of 2226 independent reflections with I≥2°(I)were collected on a GAD-4 four-circle diffractometer using Mo Ka radiation.The structure was solved by Patterson method and difference fourier synthesis,and refined by full-matrix Least-squares.Final discrepancy factor R=0.0466.All calculations were performed with a PDP 11/34 computer using SDPprograms.The coordination features of Sand Natoms of the molecule are discussed.The crystal structure of C5H5FeC5H4SO2N(C2H4CN)CH2C6H5 was determined by X-ray analysis The crystal is monoclinic,belonging to space group P21/n with unit cell dimensions.a=8.750(1),b=12.876(5),c=16.744(2)A β=94.75(1),V=1880.0A3,Z=4,Dc=1.442g/cm3.The intensities of 2226 independent reflections with I≥2°(I)were collected on a GAD-4 four-circle diffractometer using Mo Ka radiation.The structure was solved by Patterson method and difference fourier synthesis,and refined by full-matrix Least-squares.Final discrepancy factor R=0.0466.All calculations were performed with a PDP11/34 computer using SDPprograms.The coordination features of Sand Natoms of the molecule are discussed.
    The Study of Mossbauer Spectra of the Fe3O4 Mineral Agglomerates in the Sintering
    Li Zhengwen, Ma Ruzhang, Wang Shutong, Liu Ye
    1986, 7(11):  1035-1037. 
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    Mossbauer Spectra of the agglomerates are studied.The results show that the relative content of Fe3O4 and α-Fe2O3 in the agglomerates during the sintering is computed,the remained Fe3O4 is higher in the agglomerates because the(Mg,Al,Fe)3O4 has formed with metal ions Mg and Al getting into Fe3O4 lattice and replacing Fe2+ions in the sintering and there are a little or absent iron atoms in the pyroxene of agglomrates.the(Mg,Al,Fe)3O4 has formed with metal ions Mg and Al getting into Fe3O4 lattice and replacing Fe2+ions in the sintering and there are a little or absent iron atoms in the pyroxene of agglomrates.
    NMR Study on Several Polysubstituted Pyrroiesc(Ⅱ)
    Li Rao, Zhao Chengzhi, Xu Qinglun, Zhang Shuwen
    1986, 7(11):  1038-1039. 
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    13C-NMRspectra of 12 polysubstiiutcd pyrroles on 1-phenyl-2-mcthyl-3-acetyl-5-meta-nitrophenyl pyrrole derivatives were determined in this work.The resonance lines for these compounds were assigned,and the empirical substituent increments of effecting by 2-mcthyl-3-acelyl-5-mcta-nitrophenyl pyrrolinyl and it's semicarbazone on the chemical shifts of carbons in the benzene were attained.
    The Study on Photocrosslinking Reaction of Sensitized 3,4-Polyisoprene-2,6-Bis(4/-Azidobenzal) Cyclohexanone
    Huang Junlian, Yu Tongyin
    1986, 7(11):  1040-1045. 
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    This paper studied the pholocrosslinking reaction of sensitized and unsensilized 3,4-polyisoprene-2,6-bis(4'-azidobenzal)cyclohexanoncIt was found that in the system of sensitized 3,4-polyisoprenc-2,6-bis(4'-azidobenzal)cyclohexanonc,the number of double bonds decreased greatly and the content of nitrogen increased 4 to 5 times than unsensitized system.By means of IRand LCfor measurement of the photocrosslinking products and its CC14 extractives respectively,it was confirmed that the essential reaction in benzophenone-scnsitizcd system was the addition between dinitrene and the external double bonds which were activated by benzophenonc,although the cyclized reaction was the principal mode of external bonds consume.
    The Effect of Heat Treatment on Thermal, Mechamical Properties and Morphological Structure of Polyether Sulfone
    Wu Zhongwen, Wei Qingyang
    1986, 7(11):  1046-1050. 
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    In this article the influence of heat treatment on the structure and properties of rigid polyether sulforne chain has been investigated thzoughly.It was found that the glass transition temperature of the material increases nd an unusual endothermic peak appears in the transition region when is thermal-treated at a preferable temperature under its Tg(200℃).With the aid of a new designed thermal stress apparatus(TSA)we found that during the course of post-elongation recovery,plastic defermation takes place and there is almost no elastic recovery after releasing of external force for untreated sample which has the similar behavior to that of polystyrene,a typical amorphous polymeric material.However,elastic defermation takes place and there is almost no permanent set after releasing of external force for thermal-treated sample which has the similar behavior to PET,on crystallin polymeric material.The result of Electron-microscopy investigation indicates that polyether sul-fone has a new order stucture because the two phase morphology with different contrast appears in the bright field picturs and clear diffraction cycles appear in the constiucncy electron diffraction diagram.In this article the influence of heat treatment on the structure and properties of rigid polyether sulforne chain has been investigated thzoughly.It was found that the glass transition temperature of the material increases nd an unusual endothermic peak appears in the transition region when is thermal-treated at a preferable temperature under its Tg(200℃).With the aid of a new designed thermal stress apparatus(TSA)we found that during the course of post-elongation recovery,plastic defermation takes place and there is almost no elastic recovery after releasing of external force for untreated sample which has the similar behavior to that of polystyrene,a typical amorphous polymeric material.However,elastic defermation takes place and there is almost no permanent set after releasing of external force for thermal-treated sample which has the similar behavior to PET,on crystallin polymeric material.The result of Electron-microscopy investigation indicates that polyether sul-fone has a new order stucture because the two phase morphology with different contrast appears in the bright field picturs and clear diffraction cycles appear in the constiucncy electron diffraction diagram.
    Study on Acetylation of Chitin
    Yan Jun, Xu Rongnan, Xia Yan
    1986, 7(11):  1051-1053. 
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    Acetylation of chitin with acetic anhydride was investigated using p-toluene sulfonic acid,perchloric acid or a mixture of p-toluene sulfonic acid and perchloric acid as catalyst.It was found that with these methods products having high degrees of acetylation and good solubility in formic acid could be obtained.
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