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Table of Content

    24 August 1996, Volume 17 Issue 8
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    Articles
    Interactions of Diphenyltin Dichloride with Nucleotides
    LI Qing-Shan, YANG Pin, WANG Hong-Fei, GUO Mao-Lin
    1996, 17(8):  1165-1168. 
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    The interactions of diphenyltin dichloride(Ph2SnCl2)with nucleotides were studied in aqueous solutions.The new complexes of Ph2Sn(5'-AMP)·H2O, Ph2Sn(5'-CMP)·H2 and Ph2Sn(5'-GMP) were characterized by means of elementary analysis, thermal analysis, FTIR,1Hand 31PNMRspectra.In all the complexes, tin is only coordinated with the phosphate group of nucleotide, The possible structures of the new complexes are proposed.
    A Study of Adsorption of Indium with N503 Levextrel Resin
    CHEN Jian-Rong, LIN Jian-Jun, ZHONG Yi-Jun, DONG Xun-Jie, SHOU Kai-Sheng
    1996, 17(8):  1169-1172. 
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    The adsorptivity of N503 [N,N-di (sec-octyl)acetamide] levextrel resin to indium in HCl,HBr and H2SO4-NaBr media was studied.The adsorption kinetics and adsorption mechanism for N503 levextrel resin to indium in HBr medium were also discussed.The results show that the adsorption of the N503 levextrel resin to indium is carried out in pseudo first order reaction and follows freundlich isothermal adsorption equation.Studies on the adsorption equilium and infrared spectrum show that the adsorption reaction of N503 levextrel resin to indium abides by the following equation: In3++H++4Br-+2N503＝(N503)2HInBr4
    The Synthesis and Crystal Structure of Crown Ether with Heterohexaoxometalate Supermolecular Complexes
    LU Xiao-Ming, LIU Shun-Cheng, JIN Xiang-Lin
    1996, 17(8):  1173-1176. 
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    Two new supermolecular complexes of[Na(DB18C6)(CH3OH)]:W4Mo2O19·(DB18C6)·(CH3OH)(1)and [Na(DB24C8)]2W1Mo5O19(Ⅱ)were synthesized, their structures were characterized by IR,1H NMRand elementary analysis,and also determined by fourcircle X-ray diffractometer.The parameters of crystal structure of complex(Ⅱ)are :space group P21/c,α=1.8699(5)nm,b=1.9543(5)nm,c=2.2808(6) nm,β=112.87°,Z=4.It was shown that the formation of the two complexes is in different ways: DB18C8 is linked to polyoxometalate anion through C-O-Na-O-M (M= Wor Mo)long distant bonds, but DB24C8 with Na+ combined with anion by electronic interaction,It was also found that the crown ether with different radii of cavity selected different heterohexaoxometalate in which the occupation of Wand Mo is different to coordinate.
    The Synthesis and Structure of Large Crystal Cobalt Phosphate from Non-aqueous System
    XU Jia-Ning, YUAN Hong-Ming, BU Wei-Ming, SHAO Yi-Ming, SONG Tian-You, FAN Yu-Guo, XU Ru-Ren
    1996, 17(8):  1177-1178. 
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    Large single crystal of (C2H10N2)0.5 CoPO4 with novel open-framework structure was synthesized from non-aqueous system with ethylene glycol as the solvent.The crystal structure was solved by heavy atomic method and the crystal is monoclinic,space group P21/n with α=1.0410 (1) nm,b=0.8947 (1) nm,c=1.0414 (1) nm,β=90.085°,V=0.97002 (12) nm3,Z=4,Dc=1.832 mg·cm-3,R=0.063.
    Syntheses and Characterization of Rare Earth Complex with Polyaza Polycarboxylic Macrocycle Na [Ln(DOTMA)(H2O)]·2H2O
    CHEN De-Fu, JIN Tian-Zhu
    1996, 17(8):  1179-1181. 
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    The 1,4,7,10-tetraazadodecane (abbreviatedas cyclen)was synthesized according to the methods of Richman and Atkins,and the 1,4,7,10-tetraazadodecane-α,α',α",α-tetramethyl-1,4,7, 10-tetraacetic acid(abbreviated as DOTMA ) was synthesized by the reactin of cyclone with 2-chloropropanoic acid.The complexes were synthesized by the reaction of DOTMAwith rare earth chloride,and characterized by elementary analysis, thermal analysis and IRspectra.The structure forms of the complexes were expressed as Na [Ln(DOTMA)(H2O)]·2H2O, in which Ln is La, Nd, Er, respectively.
    Hydrothermal Synthesis of CepO4
    XU Yue-Hua, XU Xiu-Ting, FENG Shou-Hua, PANG Wen-Qin
    1996, 17(8):  1182-1184. 
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    CePO4 was hydrothermally synthesized in the system of K2O-CeO2-P2O5-H2O at 250℃.The factors influencing the products were investigated.The results show that lower pH, higher temperature and longer crystallizing time are favorable for the synthesis of CePO4. The products were investigated by means of XRD, IR and DTA-TG.The results showed that the product prepared by hydrothermal method is stable up to 1000℃.
    Studies on the Interaction Between Poly (I:C)and Cd2+
    HUA Er-Bing, YANG Pin, WANG Hong-Fei, YANG Bin-Sheng, ZONH Jian-Chao
    1996, 17(8):  1185-1187. 
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    The interaction of Cd2+ with the Aconfigurational doublestranded helix poly (I:C) was studied by rnelting curves,circular dichroism spectra,absorption spectra and fluorescence measurement.The results show that Cd2+ stabilizes the Aconfigurational poly (I: C) and binds to the negatively charged phosphates in poly(I: C).The binding constant of Cd2+ with poly(I:C) is(4.0±0.3) ×103 (mol/L)-1.
    Synthesis of Heteropoly Blue of Praseodymium Tungstophosphte with Keggin Structure and Studies on Their Anti-HIV Activity
    LIU Shu-Xia, LIU Yan-Yong, WANG En-Bo, ZENG Yi, LI Ze-Lin
    1996, 17(8):  1188-1190. 
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    e-and 4e-Heteropoly bule compounds of praseodymium tungstophosphate with Keggin structure were synthesized for the first time using control-potential electrolysis method, IR, UV-Vis and 31P NMRspectra were used to characterize their structures.The test of checking proliferation of MT-4 cells and their anti-HIVactivities show that these heteropoly blue compounds of praseodymium salts with Keggin structure have fairly low cell toxicity and relatively high anti-HIVactivity, The TI50 of Pr(2)and Pr(4)are 66 and 70,which demonscrate that their anti-HIVactivities are better than those of PM-29.
    Research on Modified Electrode of Conducting Polymer (Ⅱ)──Characteristic of Polypyrrole Film Doped with Heteropolyanbns
    DING Jie, DONG Shao-Jun
    1996, 17(8):  1191-1194. 
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    Polypyrrole film electrode with Co(W2O7)610- and CuW12O406-ions were synthesized in aqueous solutions, The electrode possesses a good stability and cyclic voltammetric behavior in weakly acidic or near neutral solutions.The redox of CuW12O610- ion can be catalysed by the polypyrrole film.The ESRmeasurement of the polypyrrole film with Co(W2O7)610- and CuW12O106- ions indicates that the heteropolyanions not only play the role of neutralizing electricity in the polypyrrole film,contrasted with the film containing NO3-, but also interact with the polypyrrole molecular chain to form some additive compound.The additive compound affects the electric structure of the polypyrrole film and is unstable at more positive or more negative potentials.
    Studies on Ionic-exchange Behaviour of EMD and Selective Adsorption of Lithium Ions by EMD Ionic-sieve Method
    ZHANG Bi-Quan, HUANG Chui-Quan
    1996, 17(8):  1195-1197. 
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    Fibrous electrolytic manganese dioxide(EMD) was prepared from manganous chloride solution by electrolyzing at 90~95℃with graphite anode, EMDhas the exchange properties with cations in aqueous chloride solutions,Alithium type ionic-sieve made from EMDsubstrate may be used for selective adsorption of trace lithium from sea water with an efficiency of about 90% yield.
    Micellar Electrokinetic Capillary Chromatographic Analysis of Platelet Activating Factor in Human Blood by Indirect Ultraviolet Detection
    HE Jin-Lan, LI Hui-ping, CHEN Lie, CHEN Wei-Zhen
    1996, 17(8):  1198-1202. 
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    O-Hexadecyl-and 1-O-octadecyl-sn-glycero-3-phosphorylcholine(C16-AGEPC and C18-AGEPC) in the platelet activating factor of human blood were analyzed by micellar electrokinetic capillary chromatography (MECC) with indirect ultraviolet absorption detection at 254 nm.The optimum running buffer for the separation was prepared by containing 50 mmol/Lsodium dodecy sulphate-20 mmol/Lpotassium hydrogen phthalate-10 mmol/Lborax-3mol/Lurea(pH=6.8).The separation was completed within 10 min,The detection limits of C16-AGEPC and C18-AGEPC were the same,i.e.60 ng/mL(k=3).The analytical precisions(n=6) were 2.8%~3.0% and 1.4%~1.7% for the determination with peak height and for the measurement of the migration time, respectively,The application of this method to the clinical samples was demonstrated.
    Standardization for Retention Data of Drugs in RP-HPLC──A Study of Retention Index System
    ZENG Su, LUAN Lian-Jun, WANG Si-Ju, LIU Zhi-Qiang
    1996, 17(8):  1203-1206. 
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    A retention index system based on alkan-2-ones was introduced for RP-HPLC.The effects of pH and methanol concentration in the mobile phase on RIwere examined.RI of seventy drugs and rnetabolites was determined using ODS-and phenyl-column with UVand RIDdetectors.The correlation between the lgk' and carbon number was linear from the second homologue.It has been proved that the RI decreases the variability of retention data and is suitable for the identification of drugs and the comparison of retention data obtained from different laboratories,instruments,columns,RIwas used for studying QSAR and QSRR of drugs and metabolites because there was a significant correlation between RIand lgPor π.
    Single Nerve Cell Analysis by Capillary Electrophoresis with Amperometric Detection
    HU Shen, PANG Dai-Wen, WANG Zong-Li, CHENG Jie-Ke, LI Zi-Wang, FAN You-Zhen, HU Hong-Zheng
    1996, 17(8):  1207-1209. 
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    This Paper reports the use of capillary electrophoresis (CE)with electrochemical detection to first detect the amol amount of norepinephrine (NE) and epinephrine(E) in a single sympathetic nerve cell (diameter 15~25μm ,volume 2~5pL) of rat.The home-made CEwith electrochemical detection system consists of whole cell sampling, CEand amperometric detection.The whole cell sampling involves a micromanipulator, an inverted microscope and an in jection end of the capillary.To aid cell injection, the injection end of the capillary was etched to 100μm with hydrofluoric acid.The CEapparatus consists of 30 kVdc power supply , platinum wires and a fused-silica capillary (25μm i.d., 375μm i.d.,75 cm length) filled with 25 mmol/L MES buffer solution at pH 6.5 The amperometric detector used in this experiment was a carbon fiber microelectrode, The carbon fiber having a diame ter of 8μm and a length of 0.3mm,was inserted directly into the end of the electrophoresis capillary by micropositioner and microscope,The potential on the carbon fiber working electrode was controlled to 0.7Vvs.SCEreference electrode by a potentiostat.Currents produced were measured and recorded by a picoammeter and a recorder.Sympathetic ganglia were dissected from rats.After enzymolysis the cells were isolated.The injection end of the capillary was placed adjacent to the cell using micromanipulator under the microscope,The whole cell sampling was accomplished for CEby directly drawing a cell into the tip of a capillary with electroosmotic flow and lysing the cell inside the capillary as observed under the microscope, using a micromanipulator, All separations were performed in 25 mmol MESbuffer solution using 18 kV separation potential.The amperometric detector with microelectrode was used for detecting the neurotransmitters.The results in separation and detection the amol amount of NE and Ein a single sympathetic nerve cell using this system are satisfactory.
    Simultaneous Resolution of Stability Constants and Spectra of Complex by Using Numeric Genetic Algorithm
    ZHANG Zhong-Jie, LI Tong-Hua, ZHU Zhong-Liang, CONG Pei-Sheng, SUN Yun-Pihg
    1996, 17(8):  1210-1212. 
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    The information involved in two-dimensional data is more than that involved in vector,so the treatment of the two-dimensional data has been an interesting problem.In this paper,a new method is proposed to analyze the pH-spectrophotometric data with numeric genetic algorithm(NGA).The advantage of this method is that the stability constants of complex and the absorbance curve of every component would be extracted simultaneously.This method would not be limited by the distribution of the components in the system.
    Spectra of Resonant Luminescence and Double Scattering of Selenium (Ⅳ)-iodide-crystal Violet System
    LIU Shao-Pu, LIU Zhong-Fang
    1996, 17(8):  1213-1215. 
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    The spectra of resonant luminescence(RL) ,double scattering(DS) and anti-double scattering(ADS) of selenium(Ⅳ)-iodide-crystal violet system were studied.The spectral characteristics,the effect factors and optimum conditions of the reaction have been investigated.The quantitative relations of the IRL, IADSand IDSto the concentration of selenium (Ⅳ)have been investigated.The concentration of selenium is directly proportional to the IRL,IADSand IDs in the 0~3.0μg/mL.The new analytical way for determination of trace amounts of selenium by RLand ADSwas proposed.The methods have very highly sensitivities,the detection limits for selenium (Ⅳ)are 0.11 ng/mLfor RLmethod and 0.16 ng/mLfor ADSmethod, respectively.
    Studies on Solid Surface Room Temperature Fluorescence for Determination of Five Tetracycline Antibiotics
    XIE Hong-Zhi, DONG Chuan, LIU Chang-Song, ZHAO Li-Xia, DU Xue-Qin
    1996, 17(8):  1216-1218. 
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    The solid surface room temperature fluorescence (SS-RTF)for determination of five tetracyclines on filter paper and the simultaneous determination of chlortetracycline(CTC) and tetracycline (TC) or CTC and oxytetracycline were described.Various factors of effect on RTFintensities of tetracyclines, such as pH condition, drying temperature and time of sample etc.were studied.The linear dynamic ranges, limit of detections and RSD were:2.1~205.0ng,1.3ng and 3.1 % for CTC;5.9~496.4ng,1.8ng and 2.6% for OTC;3.8~481.0 ng,3.6 ng and 2.8 % for TC;3.7~462.6ng,2.7 ng and 4.1 % for doxycycline (DOTC); 5.8~193.0ng,5.2 ng and 3.4% for methacycline (MTC), respectively.The recoveries of them in urine are from 95 % to 105%.
    Determination of Lead in Wine by the FIAS-FAAS Combination On-line Preconcentration System
    SUN Xiao-Juan, B. Welz M. Sperling
    1996, 17(8):  1219-1221. 
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    Aflow-injection on-line preconcentration and seperation procedure for flame-AASwith a microwave digestion system is described for the determination of lead at μg/Llevels in wine.The sorbent extraction preconcentration system is a micro-column (50μL) with bonded silica groups C18 as the sorbent and DDCas the complexing agent.The wine samples were digested using hydrogen peroxide as a digestion oxidizer in the microwave digestion system.An enrichment factor of 100 and a detection limit (3σ) of 3.0μg/Lwere thereby obtained.The sample throughput was 33/h for a sample loading time of 90 s with RSD 1.8 %(n=11).The recoveries of lead added in wine were 95%~103%.
    Voltammeric Determination of DNA with Doxorubicin Hydrochlorldum as Intercalator on Graphite Electrode
    FANG Yu-Zhi, LIU Sheng-Hui, HE Pin-Gang
    1996, 17(8):  1222-1224. 
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    Asynthesized 75-mer single stranded DNA (ssDNA-1) was covalently immobilized on a oxidized graphite electrode surface that had been activated using EDCand NHS.The immobilized ssDNA-1 hybridized with various concentrations of complementary ssDNA-2 in hybridization buffer containing DXH.The dsDNA/DXHsystem was formed on the electrode surface.The cathodic waves of the DXHbound to the dsDNAwith cyclic voltammetry were used for the determination of ssDNA-2.The reduction peak currents of DXHwere linearly related to the concentration of ssDNA-2 between 1×10-5 to 5×10-7 mg/mL.The determination demonstrated the method is practicable.
    Synthesis and Cyclomercuration of 1,1'-Bis[1-(arylimino) ethyl] ferrocenes
    LIU Yuan-Hong, WU Yang-Jie, YUN Hong-Ying, YANG Li, ZHU Qi-Xiu
    1996, 17(8):  1225-1230. 
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    Eleven kinds of 1,1'-bis[1-(arylimino)ethyl]ferrocenes 1 and eight kinds of mer curated products of 1,1'-bis[1-(arylimino)ethyl]ferrocene were synthesized.Their compositions and structures were confirmed by elementary analysis,IRand 1HNMR.All of them are new compounds except lc.The mercuration of compound 1 mainly produced the monoortho-mercurated products except 1b which only gave the bis-ortho-mercurated product.The yields are lower than that in the case of mono-ferrocenylketimines.The factors which influenced the mercuration were discussed.
    Synthesis of 1-Arylaminocarbonyl-3-benzylthio-4-carbethoxy(or cyano)-5-aminopyrazole
    LU Rong-Jian, YANG Hua-Zheng, ZHAO Guo-Feng, LIU Hua-Yin
    1996, 17(8):  1231-1234. 
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    1-Arylaminocarbonyl-3-benzylthio-4-carbethoxy(or cyano)-5-aminopyrazoles(3)were synthesized by the reaction of the 5-amino-3-benzylthio-4-carbethoxy(or cyano) pyrazole with the aryl isocyanate.It was found that there were great influence of the property and position of substituents X,Yon the chemical shift of H-(N2) in1H NMRspectra.By means of molecular mechanics calculations, the substituent effect on the chemical shift of H-(N2) was rationalized.The preliminary bioassay shows that some compounds have herbicidal activities.
    Synthesis of Some 4-(Un) Substituted Benzyl Piperazine-2,6-diones
    QIN Zhao-Hai, CHEN Fu-Heng, XIE Yu-Yuan
    1996, 17(8):  1235-1239. 
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    The development of several methods for the synthesis of four classes of 1,4-disubstituted piperazine-2,6-diones which have chelating effects or latent chelating effects is described.Some of them are proved to be considerably effective against P388 cells in vitro.
    Synthesis and Bioactivity of Fused Phosphorus Heterocyclic Compounds(Ⅳ)
    LU Rong-Jian, LIU Hua-Yin, YANG Guang-Fu, YANG Hua-Zheng
    1996, 17(8):  1240-1243. 
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    The Mannich-type cyclizative reaction of 5-amino-3-benzylthio-4-cyano (ethyloxycarbonyl) pyrazole with phenyl phosphonyl dichloride and the aromatic aldehyde in the presence of cation exchange resin D72 was reported.Nine 2-benzylthio-3-cyano (ethyloxycarbonyl)-5-aryl-6-phenyl-6-oxo-6-phospha-4,5,6-trihydroimidazolo[2,3e]pyrazoles were synthesized and identified as trans-configuration by means of1H NMR,31PNMR, The mechanism of the reaction was described.The preliminary biological tests show that some compounds have herbicidal activity.
    Studies on Synthesis and Conformation of Calix[4] arene Derivatives
    LU Guo-Yuan, CHEN Zhong-Jun, ZHAO Rong-Zhong, HUANG Xiao-Hua, HU Hong-wen
    1996, 17(8):  1244-1246. 
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    Six new calix[4]arenes containing different substituents[Cl, Br ,CH3,C(CH3)3] have been prepared from the cyclization of methylene bridged trimers of 4-substituted phenols and 2,6-bis (bromomethyl)-4-substituted phenols over the catalyst of TiCl4 in diglyme solvent with about 25% yield.NMR studies of new calix[4] arenes revealed that methylene protons signals appear at about δ3.40 and 4.20 as coupling two double peaks and methylene 13Csignals appear at about δ31.5.The preferred conformation of all six calix[4]arenes are cone conformation in solution.
    Studies on Synthesis and Biological Activity of N-Pyrazolinyl-α-aminophosphonates
    LONG Yun-Xian, ZHANG Ke-Sheng, QIU De-Wen
    1996, 17(8):  1247-1249. 
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    Aseries of new N-pyrazolinyl-α-aminophosphonates were synthesized by the addition of diethyl phosphite and benzyl-iminoantipyrine.Their structures were confirmed by IR,MS, 1H NMRand elementary analysis,The differences of two ethyloxyl groups in1H NMRwas discussed.The preliminary bioassay shows that some of them have a good antivirus activity on plants.
    The Instect Antifeedantal Sesquiterpenes from Celastrus Orbiculatus(Ⅱ)
    WANG Ming-An, CHEN Fu-Heng
    1996, 17(8):  1250-1252. 
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    One new antifeedantal sesquiterpene(1) along with two known sesquiterpenes lα,6iβ-diacetoxy-9β-benzoyloxy-β-dihydroagarofuran(2) and lα-acetoxy-6β-9β-dibenzoyloxy-β-dihydroagarofuran(3) were isolated from the seed oil of Celastrus orbiculatus.The structure of the new sesquiterpene was elucidated as lα,2α,8β-triacetoxy-9β-cinnamoyloxyβ-dihydroagarofuran by UV,IR,MSand 1H NMR,13C NMR,COSY,13C-1 H COSY,HMBC .
    X-ray Analysis of PLZT Solid Solution Formed under Hydrothermal Conditions
    CHENG Hu-Min, JIAO Jing, MA Ji-Ming, ZHAO Zhen Guo, QI Li-Min
    1996, 17(8):  1253-1257. 
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    PLZT solid solutions formed under different hydrothermal conditions (130~220℃,cKOH=1~5mol/L, Zr/Ti( molar ratio)=0/10~10/0,cLa=0~20%,Pb/( Z+Ti)(molar ratio) =1.0~1.7,reaction time 2 h) were investigated by means of XRD.Incorporating La3+ ion into the lattice of PZTsolid solution to substitute Pb2+ or Zr4+ and Ti4+ions was difficult under above hydrothermal conditions.The La3+could exist in the grain boundary zone or be adsorbed on the surface of PZTparticles, and in corporated gradually into the lattice of PZTwith further heat-treatment.A-site substitution was easy to occur in the tetragonal phase zone of solid solution to result in shrinkage of the cell volume of solid solution,Asite and B-site substitutions could occur simultaneously in the rhombohedral phase zone to keep the cell volume unchanging essentially.The existence of La was in favour of the formation of solid solution in the tetra-rhomb morphotropic phase boundary zone.The reaction temperature and concentration of mineralizer KOH have a significant effect on the formation and morphology of solid solution products.
    Studies on Binary Gas Solid Adsorption(Ⅵ)──Binary Gas Adsorption on Lamp Black with Different Surface Coverages
    DAI Min-Guang, MIAO Rui-Ping
    1996, 17(8):  1258-1262. 
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    The composition adsorption isotherms(ya~xg curve) for toluene-n-hexane, benzene-n-hexane,acetone-n-hexane and n-pentane-n-hexane vapor mixutres on lamp black with different surface coverages(θ)at 25℃ were measured.The experimental results indicate that the ya~xg curves approach gradually up to their binary liquid vapor equilibrium curve with increasing surface coverage.Therefore,the binary gas phase and adsorption phase at equilibrium are similarly with the binary gas liquid phase equilibrium.The composition adsorption isotherms of the four binary gases adsorption on lamp black systems are in accordancl with simulated equation of relative volatility.
    A ZINDO-SOS Study on Nonlinear Second-order Optical Properties of Phenothiazine Derivatives Substituted on Lateral Rings
    FENG Ji-Kang, GAO Xiao-Shun, XIAO Chang-Yong, SUN Chia-Chung
    1996, 17(8):  1263-1268. 
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    On the basis of ZINDOmethods,according to the Sum-Over-States(SOS) formula,the program for the calculation of nonlinear second-order optical susceptibilitiesβijk and βμ has been devised.The structuresand onlinear second-order optical properties of phenothiazine derivatives substituted on lateral rings by different substituents have been studied.It is concluded that both donor and acceptor(not too weak) substituted on lateral rings facilitate the nonlinear second-order optical susceptibility.Extending the onjugated area the nonlinear second-order optical susceptibility is increased too,and the calculated results have been explained micromechanically.
    Effect of Guanidine Hydrochloride on the Activity of RNase A in DAB Reverse Micelles
    HUANG Wen, BI Zhi-Chu, Gu Ti-Ren
    1996, 17(8):  1269-1272. 
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    The effect of guanidine hydrochloride on the activity of Bovine Pancreatic ribonuclease Asolubilized in reverse micelles formed in cyclohexane by dodecylammonium butyrate(DAB) and water has been investigated using cytidine 2',3',-phosphate as the substrate, It was noted that the enzyme entrapped in DABreverse micelles maintained more activity compared to aqueous solution at the same guanidine concentration, because protein molecule was constrained by the micellar enviroment into a conformation close to the native.Fluorescence studies showed that the degree of polarization of protein fluorescence in the micelles increased with respect to that in water which also suggested a lower mobility of the protein.
    Theoretical Studies on P14 Cluster
    FENG Jian-Nan, HUANG Xu-Ri, LI Ze-Sheng, SUN Chia-Chung, ZHANG Gang
    1996, 17(8):  1273-1276. 
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    P2+P4(Td)+P8(C2v)→P14(Cs)(A),P8(C2v)+3P2→P14(C2v)(Ⅰ)(B),P10(C2v)+2P2→P14(C2v)(Ⅱ)(C)are designed by acting P2,P4 (Td),P8(C2v)and P10(C2v)as the structural units, Using Gaussian-94 ab initio program, the four kinds of structural units and three configurations of P14 cluster[Cs,C2v(Ⅰ),C2v(Ⅱ)] are performed by full geometric optimization by choosing6-31Gbasis set.The calculated results of relative energy show that the configurations of P14(Cs) and P14(C2v)(Ⅰ)are stable,Furthermore, we design(7/2)P4(Td)→P14(D),7P2→P14(E), the relative energy shows that the structure of P14 (Cs)is stable, The results of the three structures of the P14 cluster show that the range of single bond lengths which link phosphorous atom is 0.220~0.228 nm,the range of double bond lengths is 0.200~0.202 nm, which are in accordance with the experimental values.
    A Study of Thermal Diels-Alder Reaction of Ethene with Cyclohexa-1,3-diene by Using AM1 Method
    HONG San-Guo, LI Yong-Hong, WANG Shen
    1996, 17(8):  1277-1279. 
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    UHF/AM1 molecular orbital method has been employed to study the thermal Diels-Alder reaction of ethene with cyclohexa-1,3-diene,The results showed that this reaction is exothermal,and it has two competitive routes;the activation energy of the concerted process is ll2.667 kJ/mol,and that of the rate-determining step of the biradical pathway is 78.406 kJ/mol,the biradical process has lower activation energy than the concerted one.
    Self-organization Neural Tree Applied to Structure-activity Relationship of 3-Methylfentanyl Derivatives
    FANG Jian-Hui, LU Wen-Cong, DING Yi-Min, YAN Li-Cheng, CHEN Nian-Yi
    1996, 17(8):  1280-1284. 
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    In this paper,the non-linear relationship between the characteristic parameters and analgesic activities of a series of 3-methylfentanyl derivatives was calculated by self-organization neural tree model.The results show that the performance of the self-organization neural tree is quite good and the successful classification rate is high.Therefore,we can expect that this model might be used as an effective assistant technique for the investigation of structure-activity relationship of drugs.
    The Law and Mechanism of Grinding Demulsion
    CHU Ying, LIU Pei-Yan, MA Zhan-Fang, WU Zi-Sheng, YAN Zhong, SONG You
    1996, 17(8):  1285-1288. 
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    We introduced the experimental law of grinding demulsion and discussed its basic steps:(1) The inner phase of emulsion wets the surface of grinding materials and spreads vater membrane,furtherly,liquid drops to coalesce in the course of filteration-filtering demulsion.(2) Collision among grinding materials exerts a frictional force and shearing stress on liquid drops and results in coalescence of liquid drops-grinding demulsion.
    NMR Studies on a Novel Molecular Oscillator
    SUN Xiao-Qiang, HE Ming-Yang, YANG Yang, MENG Qi, HE Guang-Yu
    1996, 17(8):  1289-1291. 
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    Anovel pseudorotaxane has been demonstrated to be efficiently self-assemblied by threading procedures from л-electron rich hydroquinone derivative and л-electron deficient bipyridinium cyclophane,The results obtained with NMRstudies show that it is possible to construct an apparently supramolecular system with potential molecular oscillator action.
    A New Chemical Oscillator in Group ⅥA:Na2S2O8-KSCN-CuSO4 System
    LIN Juan-Juan, GAO Qing-Yu, SONG Hao, HUANG Zhen-Yan, ZHAO Xue-Zhuang
    1996, 17(8):  1292-1294. 
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    A new chemical oscillator in group Ⅵ A was first discovered in the Na2S2O8-KSCN-CuSO4 system.In a batch reactor the reaction displays single-peak behavior in redox potential.In a continous stirring tank reactor(CSTR) the reaction displays sustained oscillations both in redox potential and pH.Depending upon the composition and flow rate of the input stream, we find either a low pH(pH=l~4) steady state,sustained oscillation(pH=5~6) ,or a high pH(pH=9~10)steady state.The reaction system still displays oscillation behavior when the reductant (SCN-)is in excess.The oscillatory region is very narrow in NaOHconcentration(3×10-3 mol/L<[NaOH] <1×10-2 mol/L).
    Chemisorption of H2 on Rh/SiO2
    CHEN Yao-Qiang, GONG Mao-Chu, MING Hong, ZHOU Jian-Lue, DU Zong-Ying, ZHU Xiao-Hong, GHEN Yu
    1996, 17(8):  1295-1296. 
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    Chemisorption of H2 on 3%Rh/SiO2 prepared by the impregnation of SiO2 with a solution of RhCl3·3H2Ohas been studied by infrared spectroscopy.When 7.98 kPa of ultrapure H2 exposed to 3% Rh/SiO2 reduced by H2 at 573 K for 2 h, three bands for Rh-Happeared at 1981,1888 and 1800 cm-1, respectively.By comparison with COadsorption on 3% Rh/SiO2 the bands at 1981, 1888 and 1800 cm-1 can be designated to linear-hydrogen,gemel-hydrogen and bridged-hydrogen.
    Studies on Phase of Catalyst for Butadiene Polymerization over Molybdenum Catalyst System
    XIA Shao-Wu, XIA Shu-Wei, ZHAO Ping, ZHANG Ping
    1996, 17(8):  1297-1299. 
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    This paper covered the phase of molybdenum catalyst system with hydrogenated gasoline as solvent,MoCl3(OC8H17)2 (i-Bu)2AlO-PhCH3 (m) as the catalyst.By means of Tyndall effect and electromicroscope observation, we found molybdenum was a colloid catalyst.The colloid particles were mainly congregated by MoCl3(OC8H17)2,which reacted with (i-Bu)2 AlOPhCH3(m) at the same time.In order to examine where the active centers of catalytic polyrnerization were, an ultrafiltration experiment was done by a pored filter.The result shows that the active centers existed on the surface of the colloid particles.So the whole catalytic polymerization was a heterogeneous catalytic reaction.The state of colloid particles was hardly influenced by ageing.This kind of catalyst system was a comparatively stable colloid system.
    Solid-state High-resolution Variable-temperature 13C NMR Shudy on HDI Based Main-chain Liquid Crystalline Elastomer
    CHEN Qun, YANG Guang, WANG Yuan-She, YU Xue-Hai, Kurosu Hiromichi, Andi Isao
    1996, 17(8):  1300-1304. 
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    The solid-state high-resolution variable-temperature13C NMRexperiments(including13C CP/MAS,13C PST/MAS,13C DD/MAS and contact time measurements)were carried out on a main-chain liquid-crystalline polyurethane elastomer based on poly(tetramethylene oxide)(PTMO),hexamethylene diisocyanate(HDI) and 4,4'-bishydroxyethyloxybiphenyl(HB2)from room-temperature to 96℃.The HDIand HB2 segments which play the role of hard segmehts of the elastomer were found to be crystalline.The inter-molecular or inter-segmental hydrogen-bonds formed between the carbonyl group and the NHgroup were found to gradually decompose with the increasing of temperature,Asecondary transition of the HB2 crystal was observed at temperatures well below the meltingpoint of the sample.
    Crystal Structure and Its Transition for Poly(aryl ether ketone ketone) s(Ⅰ)
    KE Yang-Chuan, WU Zhong-Wen, ZHENG Yu-Bin, JI Xiang-Ling, YANG De-Cai
    1996, 17(8):  1305-1309. 
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    Poly(aryl ether ketone ketone)s (PEKK) was a high-performance engineering plastics, By means of Wide Angle X-ray Diffraction(WAXD)and DifferentiaI Scanning Calorimetry( DSC) methods, PEKKsamples crystallized in solvent induction, from glass state and from melting state were studied.Crystal formsⅠand Ⅱfor PEKKwere found.The formation of crystal formⅡwas dependent on thermal history and solvent induction, and this form Ⅱhad melting point 10 ℃ or so lower than that of formⅠcrystallized from glass state.All PEKKsamples had low melting peaks which were relevant to the polarization of PEKKmolecular chain, while they had nothing to do with thermal history.The heat of fusion for PEKKlow melting peaks accounted for percentage of 2 to 10 or so of the whole heat of fusion, And PEKKhas its equilibrium melting point of 409℃.
    Isolation and X-ray Crystallographic Stucture of Cyclic Tetramer Based on Bisphenol A and o-Phthaloyl Dichloride
    JIANG Hong-Yan, LIU Tian-Xi, CHEN Tian-Lu, MO Zhi-Shen, XU Ji-ping
    1996, 17(8):  1310-1313. 
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    The polycrystalline powder of the cyclic tetramer based on bisphenol Aand o-phthaloyldichloride has been prepared by recrystallization from nitrobenzene and its crystalstructure has been determined by Wide-Angle X-ray Diffraction( WAXD ).The unit cell is orthorhombic and its dimensions α=0.967 b=0.8699 nm,c=2.0859 nm.Space group belongs to Pmmm,With two tetramers per unit cell, the crystal density is 1.36 g·cm-3.Indices of crystal diffraction peaks are also detailed in the present work.
    Cationic Polymerization of α-Pinene Initiated by AlCl3/SbCl3──Studies on the Nature or the Initiating Species
    LU Jiang, LIANG Hui, ZHANG Ren-Jun, DENG Yun-Xiang
    1996, 17(8):  1314-1318. 
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    The effects of the preparation methods of the AlCl3/SbCl3 binary catalyst and the proton trap 2,6-ditert-butyl-4-methyl pyridine(DTBMP)on the cationic polymerization of apinene were investigated respectively.The results showed that, if AlCl3 and SbCl3 were melted to form the combined catalyst,its initiating activity was higher than that of the catalyst obtained by simply mixing of AlCl3 and SbCl3.α-Pinene was hardly initiated by the simple combination of AlCl3 and SbCl3 at-78℃,howeve,the melted binary catalyst system led to a fast polymerization even at such a low temperature,The proton trap DTBMPhad no obvious effects on the AlCl3/SbCl3 catalyzed polymerization in term of the rate and the molecular weight distribution.These results indicated that new initiating species which was different from protonic species H⊕ in nature was generated by the reaction of AlCl3 and SbCl3.Furthermore,the reaction of AlCl3 and SbCl3 was examined by 27Al NMRspectrum.No signal was observed in the 27Al NMRspectrum of AlCl3 alone system because of its poor solubility in the used solvent (toluene), but there appeared a strong absorption in the spectrum of AlCl3/ SbCl3 binary system,and the chemical shifts unchanged before and after the polymerization.These show that a new Al-containing compound, soluble in toluene,was generated by AlCl3 and SbCl3 to initiate the polymerization,and that the metal atom adding to the monomer is not Al but Sb in the initiating reaction.The proposed initiating cation was[SbCl4]⊕,and the counter anion was[Al2Cl7]Θ.
    Configurational Statistics of Model Polymer Loop
    WU Da-Cheng, DU Peng, KANG Jian
    1996, 17(8):  1319-1321. 
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    A polymer chain in which two ends are attached at an interface boundary physically or chemically is called as a polymer loop.Based on the normal random walk(NRW)in the simple cubic lattice,the available conformational number C11(3)(N)of a model polymer loop with the chain length Ncan be obtained from the available conformational number of the corresponding polymer tail.It was shown that the number C11(N)≈6N/2(6лN3)1/2, where 6 Nis the conformational number of a free chain with the length N.The computer ""experiments"including the exact enumeration and the Monte Carlo simulation were used for the comparison with the theory.This result gives a formal reference frame to compare with the conformation of the more complicated model or the real polymer loop.
    Synthesis and Properties of Poly (aryl ether ketone)s Containing meta-Phenyl Links
    LIN Quan, ZHANG Wan-Jin, WU Zhong-Wen, YIN Jiu-Mei
    1996, 17(8):  1322-1324. 
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    A series of poly(aryl ether ketone)s containing meta-phenyl links are synthesized,DSC and wide-angle X-ray scattering,etc.are used to study the general properties of the polymers.With the increasing of meta linkage monomer percentage,the melting temperature decreases sharply at first,then rises steadily,the glass transition point keeps a stable value,and crystallinity and crystallizing rate are reduced.Apart of amorphous film of the polymer is annealed at different temperatures.DSCscan shows that besides Tm,a new melting peak( T'm)at low temperature appears.And with heat treating temperature rising,T'm shifts to high temperature, and Tm keeps a stable value.
    The Stacked Polymer Chains on the Surfaces of Polystyrene Microparticles
    XU Wei, CHEN Dian-Yong, HUA Zhong-Yi, LU Xu-Liang, HU Jian-Hua, FU Shou-Kuan
    1996, 17(8):  1325-1326. 
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    Polystyrene microparticles prepared by microemulsion free-radical polymerization,have been found to be much different from ordinary polystyrene,but their structures still remain unknown,Therefore we use the scanning tunneling microscope (STM) to investigate them.It is found that at least in some regions of the polystyrene surface,the polymer chains are orderly stacked without entanglement.It is also found that the oagulation of polymer chains can be varied with different regions.The existence of the orderely-stacked polymer chains might be the reason why the polystyrene microparticles have different properties from the ordinary atactic polystyrene.
    Studies on Novel Acrylic Acid Crosslinked Chitosan Pervaporation Membrane(Ⅱ)──Pervaporation Separation of Ethanol-Water Mixtures
    ZHONG Wei, LI Wen-Jun, GE Chang-Jie, CHEN Xin
    1996, 17(8):  1327-1329. 
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    Anovel acrylic acid crosslinked chitosan membrane was prepared through a homogeneous solution reaction and its pervaporation separation properties of ethanol/water mixtures were investigated.The selectivity of chitosan membrane was remarkably improved by crosslinking in the separation of ethanol/water mixtures and it highly depends on the preparing conditions and increased with temperature increasing.When the ethanol in feed is above 50% (percentage by weight),the water in permeate is no less than 98%.
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