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Chinese Journal of
Magnetic Resonance
(Quarterly, Started in 1983)
Editor-in-Chief: LIU Mai-li
Sponsored by
Wuhan Institute of Physics and Mathematics, CAS
Published by Science Press, China
Distribution Code: 38-313
Pricing: ¥ 80.00 per year
Current Issue
       Volume 11 Issue 2, 05 June 1994 Previous Issue   Next Issue
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    NMR STUDIES OF PYRIDINE -ENSOLUBLE SOLID OF VIBRAIN AND ITS HYDROCRACKING PRODUCTS
    Yang Baolian, Li Liyun, Ye Chaohui, Zhang PengZhou, Xu Xiufeng
    Chinese Journal of Magnetic Resonance, 1994, 11(2): 119-126.  
    Abstract     HTML ( )   PDF(363KB)
    Pyridine -insoluble、THF-insoluble solids of bydrocrachng products of vitrain pyridine-insoluble solid and itself were investigated by solid state 13C CP/MAS NMR technique.From the measurements, twelve structural parameters of carbon skeleton were obtained Benzene-soluble subfraction of hydrocracking products were investigated by one and two dimensions 1H and 13C liquid NMR techniques.Their 1H and 13C spectra were assigned.The avcrage molecular structures of these fractionswere obtained.
    PALASMA TREATMENT OF POLYVINYLIDENE FLUORIDE AND THEIR ESR INVESTIGATION
    Zhan RUIYUN, Liu Guizhen, Liu Xieshu, Zhu Yufen
    Chinese Journal of Magnetic Resonance, 1994, 11(2): 127-132.  
    Abstract     HTML ( )   PDF(365KB)
    The plasma treatment of polyvhylidene fluoride (PVF2)films was carried out in a capacitively coupled reactor with external electrodes.The gel content of PVF2 treated in various conditions,their shear strength and the contact angle of water on the surface of PVF2 were mcasured.ESR investigation of the free radicals produced in the process of plasma treatment,indicates that the incrcase of the unsaturated bonds in molecules and highly crosslink reaction were in favour of the adhesion of PVF2.
    NUCLEAR RELAXATION STUDIES OF MOLECULES PHYSISORBED ON CHARCOAL,ALUMINA AND SILICA GEL
    Xue Yi, Du Youru, Ye Chaohui, Kong Yuhua
    Chinese Journal of Magnetic Resonance, 1994, 11(2): 133-140.  
    Abstract     HTML ( )   PDF(439KB)
    Electron-nuclear dipolar interaction and spin-diffusion play very important roles in the relaxation processes of molecules adsorbed on solids containing surface eleetrons, such aS charcoal,alumina and silica gel.According to this relaxation rnechanism,the relation between spin-lattice relaxation time(T1e)and correlation tim-(τc)was obtainted:T1e,-k(τc/1+ω02τc2)1/2,k is a con-stant for a given solid. It was found that the relaxations of toluene adsorbed on silica gel were interpretted well by this formula, The correlation times at dirrerent temperatures and the activqtion energy(Ea=15.0kJ/mol) of methyl group in toluene adsorbed on silica gel were obtained.The correlation times are in the range of 3.56×10-9-5.76×10-8s during 374 K and 240 K.
    RADICAL INTERMEDIATES GENERATED IN PHOTOCATALYTIC OXIDATION OF SOME ORGANIC COMPOUNDS CONTAINING NITROGEN ATOMS
    Chen Ciping, Lu Daohui, Xu Guangzhi
    Chinese Journal of Magnetic Resonance, 1994, 11(2): 141-147.  
    Abstract     HTML ( )   PDF(368KB)
    Radical intermediates generated in photocatalytic oxidation of some organic com-pounds containing nitrogen atoms such as butylamine,piperidine, pyridine etc,were detected by spin trapping technique. The ESR spectra of N-eentered radical adduct and C-centered radical adduct were observed.Experiment results reveal that these radicals are participants in the inital steps of photodegradation of thesc com-pounds,A mechanism which is consistent with the observation of these radical species is elucidated.
    THE ANALYSIS OF ONE AND TWO DIMENSION SPECTRA OF POLYETHERIMIDE (YS-30)
    Zhou Zinan, Sun Zhenhua, Wu Shengrong, Feng Zhiliu, Gao Xinfeng, Xiao Yanwen, Wu Yijie
    Chinese Journal of Magnetic Resonance, 1994, 11(2): 149-155.  
    Abstract     HTML ( )   PDF(399KB)
    Polyetherimide(YS-30)is one of the soluble polyimides. This paper presents the re-sults of our study on its 13C NMR,1H NMR,H-H COSY and C-H COSY spectra. On this basis the assingments of these spectra are very satisfactorily obtamcd.Hence the chain structure of the polymer has been recongnized clearly.
    MAS NMR STUDY ON THE EFFECT OF PALLADIUM ADDITION ON SAPO-5 MOLECULAR SIEVE
    Xiao Tiancun, An Lidun, Wang Hongli, Yang Nianhua, Yuan Hanzhen, Qiu Jianqing
    Chinese Journal of Magnetic Resonance, 1994, 11(2): 157-163.  
    Abstract     HTML ( )   PDF(417KB)
    SAPO-5 molecular sicve bas been synthesized by hydrothermal method.Palladium is supported on it by adding Pd salt solution (Pd(NH3)4Cl2 and H2PdCl4)into the mixture gel of SAPO-5 before crystallizzation in order to obtain bifunctional catalyst.The result of X-ray diffraction reveals that the introduction of palladium salt in the mixture gel does not deprcss the formation of SAPO-5. However,when palladium is added in the form of Pd(NH3)4Cl2, there intergrows a little SAPO-34 in the product.MAS NMR results show that the addition of palladium obstructs silicon to enter the framework and thus makes a more symmetrical coordination environment of alumini-um and Causes partialy decomposition and polymeriZation of the template in SAPO-5.The reaction of the template during crystallization differs with the palladium precur-sors.31P MAS NMR result shows that the addition of palladium salt in the mixture gel has little influence on the coordination environment of phosphorus in the framework.
    STUDY OF 2D NMR OF TOW DITERPENES FROM TRIPTERYGIUM WILFORDII HOOK.F
    Fu Mengmeng, Zhou Xiaoxian, Xie Dilin, Deng Fuxiao, Wang Hanqing
    Chinese Journal of Magnetic Resonance, 1994, 11(2): 165-172.  
    Abstract     HTML ( )   PDF(418KB)
    Two diterpenes were isolated from tripterygium wilfordii Hook.F.The structures were deduced using various 2D NMR techniques (H-H COSY,HETCOR, COLOC).Analysis of 1H and 13C NMR spectra of 1 and 2 has all owed unambiguous chemical shift assignments of all protons and carbons of these compounds.
    THE STUDIES ON PARAMAGNETIC IONS COORDINATED TO SOME AMINO ACIDS BY NMR T1 METHOD
    Hu Jiehan, Qu Ming, Xiuwen, Xu Yongting, Yang Kaihai
    Chinese Journal of Magnetic Resonance, 1994, 11(2): 173-180.  
    Abstract     HTML ( )   PDF(474KB)
    The influence of paramagnetic ions, Fe3+ and Cu2+ on relaxation time T1 of amino acids which are structural units of peptides has been investigated in this paper.The for-mula only for monospecies system of chemical molecule and metal ion has been ex-tended to polyspecies system and the system in which there are chemical exchanges. The linear relations of paramagnctic relaxation rate(R1p) and concetration of metal ions (CM) have been elucidated and demonstrated.The relations between the slope of curves and coordinating ability and concentration of ligands have been discussed.
    THE SEPARATION OF HETERONUCLEAR DIPOLAR RELAXATION IN MACROMOLECULE
    Miao Xijia, Hu Jiehan, Han Xiuwen
    Chinese Journal of Magnetic Resonance, 1994, 11(2): 181-186.  
    Abstract     HTML ( )   PDF(369KB)
    It is proposed that only the heteronuclear cross relaxation rates between 13C and 1H,which are only dependent on the diporlar relaxation,are used to investigate the mo-lecular internal motions,The new method is more reasonable than the conventional one in theory where the nuclear longitudinal relaxation time T1,transvcrse relaxation T2 and NOE factor η are used to study the molecular internal motions. The general formu-la separating the contribution of dipolar relaxation to the total 13C spin relaxation is set up. It can be applied not only to small molecules inside extreme narrowing condi-tion but also to macromolecules outside extreme narrowing.
    THE STUDY OF 3-FORMHYDRAZONE-RIFAMYCIN SV AND ITS ISOMER
    Wang Zuoqin, Wang Gulfang, Gu Yushan
    Chinese Journal of Magnetic Resonance, 1994, 11(2): 187-194.  
    Abstract     HTML ( )   PDF(409KB)
    Two samples(1#,2#)of 3-formhydrazone-rifamycin SV produced by fermentation and chemieal modification have different physical and chemical properties.In this paper,their structures were determined by various kinds of NMR spcctra, such as 1H,13C,DEPT,1H-1H COSY,1H-13C COSY and LR 1H-13 C COSY in inverse mode, and by the absorption spectra of IR and UV-Vis.It was found that the two samples were the main product of amide mode (1#) and the isomer of iminol mode (2#). Based on the results of experiments,the isomerization of sample 1# was discussed.
    STUDY OF THE ISOTOPE EFFECT ON 14N RELAXATION IN DMF/H2O AND DMF/D2O SYSTEMS
    Li Ming, Mao Xian
    Chinese Journal of Magnetic Resonance, 1994, 11(2): 195-200.  
    Abstract     HTML ( )   PDF(383KB)
    In the present paper,the dynamic isotope effect of 14N relaxation of DMF/H2O(D2O) system is reportcd.The 14N rclaxation times of DMF in DMF/H2O and DMF/D2O systems have been measured through all composition range (mole fraction of DMF from 0 to 1).The solvent isotope effect on relaxation and the factors affecting the quadrupole relaxation are discussed.The results suggest that in the given system there is a close relationship between the 14N relaxation and the kinetics of solvent water.Under infinite dilutions,the kinetics of the solute molcculcs are controlled complctely by the solvent molecules.
    LASER MAGNETIC RESONANCE USING THE FARADAY EFFECT
    Ding Hongbin, Wang Yi, Luo xiao, Lin Jinxiu
    Chinese Journal of Magnetic Resonance, 1994, 11(2): 201-206.  
    Abstract     HTML ( )   PDF(352KB)
    The Faraday effect was used in laser magnetic resonance for improvement of the signal to noisc ratio,Both theoretical analysis and the experimcntal results are given in this paper.The results show that the signal to noise ratio was improved in more than one order.
    STUDIES ON REACTIONS OF TRANSITION-METAL HYDRIDES WITH TETEROCUMULENES Ⅲ. An ESR Evidenee for Paramagnatic Zirconium Species Generated during the Reaction of Cp2Zr(H)Cl with RNCS
    Wang Mei, Bei Meizhi, Guo Hefu
    Chinese Journal of Magnetic Resonance, 1994, 11(2): 207-210.  
    Abstract     HTML ( )   PDF(240KB)
    The reaction process of Cp2Zr(H)Cl with RNCS (R=C6H5,c-C6H11,n-C4H9) has been detected by ESR method. The ESR results show that in the process the Zr-H bond deaved homolytically and a transient Zr(Ⅲ)species is formed. The reactions oeeurred via a radical mechanism.
    STRUCTURAL ANALYSIS OF POLYCYCLIC AROMATIC HYDROCARBONS EDRIVED BY13C NMR SPECTROSCOPY
    Yan Baozhen, Yuan Hancheng, Yang Heli, Qi Hua
    Chinese Journal of Magnetic Resonance, 1994, 11(2): 211-217.  
    Abstract     HTML ( )   PDF(320KB)
    In this article three methods(inverse gated dec,J-modulated spin-echo and 2D-J-resolved) for measuring the protonated and non-protonated carbons were dis-cussed and compared. The average molecular parameters of three kinds of polycyclic aromatic hydrocarbons derived from petroleum and coal were independently calculated by three methods,and the structure of three complex mixtures were primarily analysedand discussed.
    2D NOESY EXPERIMENTAL PROBLEMS OF MEDIUM-SIZED PEPTIDES
    Zhang Yibing, Yu Yihua, Shen Wei, Wang Qiwen
    Chinese Journal of Magnetic Resonance, 1994, 11(2): 219-222.  
    Abstract     HTML ( )   PDF(237KB)
    The main difficulty in 2D NOESY of mcdium-sized peptdes is lacking of cross-peaks, espccially in the region related with NH, For solving this problem, these authors use a mixed solvent,CD3OD/H2O, to dissolve peptides,which allows NMR measurements at low temperature.The increased viscosity of solution and the correlation times by low-temperature measurements made a lot of intra-and inter-residue NOES observable, which helped us unambiguously complete the assigmnents of a nonapeptide and an undccapcptide, and further in calculation of H-Hdistances.