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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
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       Volume 6 Issue 2, 05 June 1989 Previous Issue   Next Issue
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    T1 MEASUREMENT UNDER STRONG SOLVENT SIGNAL SUPPRESSION
    Yao Shenggen, Huang Yongren
    Chinese Journal of Magnetic Resonance, 1989, 6(2): 129-135.  
    Abstract     HTML ( )   PDF(387KB)
    In the normal methods of T1 measurement, say IR method, problems of dynamic range will arise when a strong solvent signal and weak mean signals are present together, which will reduce the accuracy of T1 measurement and it is quite difficult to combine the normal T1 experiments with available methods of solvent peak suppression. In order to solve this problem, a modified IR method is provided in this paper to measure T1 with suppression of strong solvent peak. Theoretical explanation, calculation and experimental results are given. It is proved that the accuracy of this new method is the same as the normal IR experiment.
    THE STUDIES OF ELECTROCHEMISTRY OF RCCo3(CO)9 AND ESR SPECTRA OF RCCo3 (CO)9·
    Sun Shouheng, Meng Qingjin, You Xiaozeng, Qian Yue, Bu Xiuren
    Chinese Journal of Magnetic Resonance, 1989, 6(2): 137-142.  
    Abstract     HTML ( )   PDF(124KB)
    Three kinds of RCCo3 (CO)9 and their radicals have been studied with electrochemistry and ESR spectra. The reduction of RCCo3 (CO)9 are related to the nature of R and RCCo3 (CO)9· are stable at room temperature. Based on the symmetry analysis of MO, the ESR spectra of cluster radicals are discussed in detail. The sign of hyperfine coupling constant and the nature of the orbital occupied by unpaired electron are determined. Furthermore, the spin density on 3d orbital and 4s orbital of cobalt are calculated from experimental results.
    THE NMR SPECTRA AND STRUCTURE OF 2-CARBOXYETHYL TRIPHENYL PHOSPHONIUM BROMIDE
    Li Chunfang, Hong Liang, Lin Shoutian
    Chinese Journal of Magnetic Resonance, 1989, 6(2): 143-146.  
    Abstract     HTML ( )   PDF(224KB)
    In this paper, 1H, 13C, and 31P-NMR spectra of 5 bromide phosphonium salts of general formula (Ph3 PCHRCHR CO2H)Br were observed. 1H, 13C, and 31P chemical shifts and 31P-13C coupling constants were determined. The relationship between molecular structure and NMR parameters are discussed.
    MAGNETIC RESONANCE STUDY OF MIXED CONDUCTOR Li1+xV3O8 (x=0. 1) CONTAINING DSPP
    Cui Wanqiu, Chen Wen
    Chinese Journal of Magnetic Resonance, 1989, 6(2): 147-154.  
    Abstract     HTML ( )   PDF(500KB)
    The electric property and magnetic resonance of mixed conductors Li1+xV3O8 (x=0.1) containing DSPP were studied. By AC measurement, the maximum of total conductivity for sample containing about 6 mol% α-Al2O3 was four or six times to that of pure Li1+xV3O8 (x=0.1) at room temperature.
    That the addition of DSPP increases the electron density of the sample and electronic and ionic transport frequencies, decreases Li+ ionic transport activation energies i e., increases total conductivity of the sample was proved by ESR and NMR qualitative and quantitative analysis of the samples.
    The increment of the total conductivity mainly depends on the contribution of the Li+ ionic conductivity, the electronic conductivity has a definite influence on it, too.
    1H-NMR SEMI-QUANTITATIVE ANALYSIS OF THE EDIBLE OILS
    Du Dingzhun, Qian Shengqiu, Gao Meifang
    Chinese Journal of Magnetic Resonance, 1989, 6(2): 155-162.  
    Abstract     HTML ( )   PDF(471KB)
    1H-NMR semi-quantitative determination of the edible oils was carried out with necessary adjustments of the partial peak integrations in order to correct the interference of the CCH2C strong peak to the neighbouring weak ones. The amount of each functional group, ratio of quantities among various functional groups, esterification degree, unsaturation degree, average length of the saturated carbon chain, average carbon numbers in the combined fatty acids and average molecular weight per mole of oils were calculated.
    SOLUTION CONFORMATION OF TETRANDRINE
    Pan Jingxian, Zhao Jicang, Han Guiqiu, B. Arison, Y. K. Lam, P. Rinald
    Chinese Journal of Magnetic Resonance, 1989, 6(2): 163-168.  
    Abstract     HTML ( )   PDF(305KB)
    Solution conformation of tetrandrine was studied by NMR 1H NOESY and 1H-13C HETCOR. The success in interpreting all NMR observations in terms of the x-ray crystal diagram is compelling evidence that the solution and solid state conformations are essentially the same.
    INVESTIGATION OF HYDRAZONE-AZO TAUTOMERISM OF PYRIDONE AZO DYESTUFFS I The Application of Nuclear Magnetic Resonance For Identification of the Configurations
    Peng Qingji, Zhang Mingjia, Li Mujie, Gao Kunyu, Cheng Lubai
    Chinese Journal of Magnetic Resonance, 1989, 6(2): 169-176.  
    Abstract     HTML ( )   PDF(509KB)
    The 13C NMR spectra of seven azo dyes derived from pyridones were measured. The assignment of the peaks was carried out with the aid of Selective Insensitive Nuclear Enhanced by Polarization Transfer technique (SELINEPT). It has been pointed out that the phenomenon of colour-change caused by acid-base is due to the shift of equilibrium in hydrazone-azo tautomerism according to the influence of pH values upon 13C chemical shifts, 1H NMR spectra and UV-VIS absorption spectra. The enhancement of acidity and basicity is in favour of hydrazone and azo forms respectively. The different structures of the pyridone dyes change their colour at quite different pH values.
    A 1H SPIN-DIFFUSION STUDY ON THE DOMAIN STRUCTURE OF POLYURETHANE ZWITTERIONOMER
    Chen Qun, Wang Yuanshen
    Chinese Journal of Magnetic Resonance, 1989, 6(2): 177-182.  
    Abstract     HTML ( )   PDF(331KB)
    The 1H spin-diffusion process of a series of polyurethane zwitterionomers was investigated by a modified Goldman-Shen pulse sequence on a solid NMR spectrometer. The Fickian's diffusion equation was solved according to appropriate boundary and initial conditions. The data treatment was greatly simplified by doing some reasonable assumptions and omissions. The domain sizes of two samples with different degree of ionization were obtained and the influence of ionization on the morphology of the samples is discussed.
    RESEARCH ON THE PHOTOREDUCTION REACTION OF PARAQUAT SALTS WITH iso-PROPYL ALCOHOL
    Zhou Jianwei, Chen Dewen, Yang Yukun, Xu Guangzhi
    Chinese Journal of Magnetic Resonance, 1989, 6(2): 183-186.  
    Abstract     HTML ( )   PDF(259KB)
    The homogeneous photoexcited electron-transfer of PQ++-isopropyl alcohol systems in benzene solution was studied by means of spin trapping-ESR technique. Results show that PQ++ may be reduced, by the free radical (CH3)2ĊOH, to a free radical PQ·+; the rate of electron transfer can be accelerated greatly when benzophcnone is added to the photoreaction systems.
    ESR STUDY OF PHOTOLYSIS IN CIS-DICARBONYL (BIDENTATEN-DONOR LIGANOL) RHODIUM(Ⅰ) Tetraphenyl Borate Coordination Compounds
    Ji Haixing, Yuan Guoqing, Xu Guangzhi, Chen Rongyao
    Chinese Journal of Magnetic Resonance, 1989, 6(2): 187-192.  
    Abstract     HTML ( )   PDF(405KB)
    Active intermediate produced during photolysis of[Rh(CO)2Cl]2 and eight cis-dicarbonyl (didentate N-donor ligand) Rh (Ⅰ) tetraphenyl borate[Rh(CO)2 (Chel)] Bph4 were investigated by combining spin trapping technique with ESR. The results show that the primary process of photolysis in[Rh(CO)2Cl]2 is homolytic cleavage of the Rh-Rh bond to produce Rhodium-centered free radicals. They can be trapped by PBN, ND and TBN. And the photolysis of cisdicarbonyl (bidentate N-donor ligand) Rhodium (Ⅰ) tetraphenyl borate produced ph radicals of Bph4 anion, and stability of the spin adducts are related to the bidentate N-donor ligand.
    13C-NMR STUDY OF HUMIC ACID SOLUTION FROM SOIL
    Hau Shiying, Dou Sen, Zhu Tao
    Chinese Journal of Magnetic Resonance, 1989, 6(2): 193-200.  
    Abstract     HTML ( )   PDF(498KB)
    We carried out a 13C NMR study of humic acid solution from Brown forest soil and Meadow soil under different conditions. The results have shown that the best signal-to-noise ratios in a given time can be obtained by using a large number of transients spaced at short intervals, rather than a smaller number spaced at longer intervals. This is adaptable to semi-quantitative determination of carbon types.
    A STUDY OF RELATIONSHIP BETWEEN THE STRUCTURE OF CUPPERIC COMPOUNDS AND THEIR ESR TENSORS
    Lin Qingsong
    Chinese Journal of Magnetic Resonance, 1989, 6(2): 201-208.  
    Abstract     HTML ( )   PDF(467KB)
    A linear correlation of g and A of cupric ion were found for some copper compounds of particular ligands. Relationships between the correlation and structures of coppercontaining compounds have been examined. It is indicated that the relation is concerned with molecular symmetry and properties of a bonding molecular orbit. It is shown that a higher symmetry and a lower covalency of the copper-ligand bondings result in increasing of g and decreasing of A absolute value. It is also shown that there is a linear relation between g vs. β12 and A vs. β12, respectively, for some Cu (Ⅱ)-compounds. By means of experimental values of gand A, an empirical method used to estimate approximate values of β12 in molecular orbital coefficients is introduced.
    THE HYDROGEN TRANSFER OF GOSSYPOL AND ITS DERIVATIVES IN DIFFERENT SOLVENTS
    Yang Weiman, Shi Xiaoyu, Yang Tianxiang, Cheng Yongtai, Liu Fuguang
    Chinese Journal of Magnetic Resonance, 1989, 6(2): 209-220.  
    Abstract     HTML ( )   PDF(617KB)
    In this paper, the hydrogen transfer of gossypol and its imino derivatives (dianilinogossypol, dipyrimidinyliminogossypol and di-n-butyliminogossypol) in various solvents (CDCl3,DMSO-d6,C6D6,CD3COCD3 and DMF-d7) under different acidic or basic conditions was shudicd by 1H NMR method. Results show that, three different tautomers existed for each of the above mentioned gossypol imino derivatives, Moreover, the forms of these three tautomcrs are interchangable or co-exist in the same solvent under different conditions.
    THE 31P NMR SPECTRA OF 4,5-DIOXO-2-THIO-1,3,2,4-DIAZADIPHOSPHOLANE DERIVATIVES
    Li Guowei, Cheng Leifeng, Chen Ruyu
    Chinese Journal of Magnetic Resonance, 1989, 6(2): 221-224.  
    Abstract     HTML ( )   PDF(261KB)
    It was found from the 31P NMR spectra that there were cis-and trans isomers in 4,5-dioxO-2-thiO-1,3,2,4-diazadiphospholanes. The chemical shifts of the cis-isomer appeared at highfield with larger 2JPP coupling constant and the trans-isomer at lowficld with smaller coupling constant. It was explained in terms of van der Waals action and conjugated(P→d) π system. The relationship between the 31P NMR chemical shifts and substituent in phenyl is also discussed.
    THE STUDY OF THE 1H-NMR OF β,β'-DIAMINOPINACOLS
    Wu Caiyu, Feng Juncai, Zhou Zhaolin, Shen Wenbin, Chen Weixin
    Chinese Journal of Magnetic Resonance, 1989, 6(2): 225-230.  
    Abstract     HTML ( )   PDF(304KB)
    The configurations of β, β'-Diaminopinacols were discussed. The stcr-eo-isomers were determined with 1H-NMR. Comparison of the 1H-NMR at room temperature and lower temperature proved the results.
    2D-NMR STUDIES ON STRUCTURES OF 5-FLUOROURACIL DERIVATIVES
    Qiu Feng, Li Liyun, Zhou Yuanzhong, Zhou Nianen, Qian Baogong
    Chinese Journal of Magnetic Resonance, 1989, 6(2): 231-238.  
    Abstract     HTML ( )   PDF(400KB)
    2D-NMR, developed in recent ten years, plays an important role in studying structures of organic molecules. four new compounds of 5-fluorouracil derivatives were thoroughly studied by homo-and heteronuclear chemical shift correlation, heteronuclear relayed coherence transfer, and long rangecoupling heteronuclear relayed coherence transfer, and long range coupling heteronuclear chemical shift correlation spectroscopies. The structures and assignments of their 1H, 13C resonances were determined.
    STUDY OF 13C-NMR SPECTRA FOR THE COMPOUNDS OF 1-(4-PYRIDINE ACYL)-4-ARYL THIOSEMICARBAZIDE AND 3-(4-PYRIDINE)-4-AROMATIC-1,2,4-TRIAZOLINE-5-THIONE
    Song Maosen, Liu Peiqi, Zhang Ziyi, Yang Kexin
    Chinese Journal of Magnetic Resonance, 1989, 6(2): 239-244.  
    Abstract     HTML ( )   PDF(365KB)
    The carbon-13 NMR spectra of 1-(4-pyridine acyl)-4-phenyl thioscmicarbazide, 1-(4-pyridine acyl)-4-p-chlorO-phenylthiosemicarbazide, 1-(4-pyridine acyl)-4-p-bromo-phenylthiosemicarba/ide, 3-(4-pyridinyl)-4-phenyl-1, 2, 4-triazoline-5-thionc, 3-(4-pyridinyl)-p-chloro phenyl-1, 2, 4-triazoline-5-thione, 3-(4-pyridinyl)-p-bromo phenyl-1, 2, 4-triazoline-5-thione and their derivatives were studied in this paper. The chemical shifts of various carbon resonance peaks were assigned by the proton-noise decoupling, Off-resonance, APT-technique, and use of empirical methods. At the same time, the substituent effects of 4-hydrazide in monosubstituted pyridinc were obtained. These parameters are Z42 (Z46) 0.1ppm Z43 (Z45)-3.3ppm and Z44 3.9ppm (solvent:polysol; reference:TMS).
    A RETRIEVAL SYSTEM AND METHOD OF COMPOUNDS AND THEIR NMR SPECTRAL DATA
    Jiang Dazhi
    Chinese Journal of Magnetic Resonance, 1989, 6(2): 245-250.  
    Abstract     HTML ( )   PDF(386KB)
    The fundamental structure and the applied methods of retrieval system in the carbon-13 NMR data bank established by the author[3] arc described. For the molecular structural discrimination, a pre-retrieval process was adopted, and a set of parameter-retrieval methods was developed in this work.
    THE TECHNIQUE OF SELECTIVE INEPT AND ITS APPLICATION ON A FX-90Q SPECTROMETER
    Zhang Minjia, Peng Qinji
    Chinese Journal of Magnetic Resonance, 1989, 6(2): 251-254.  
    Abstract     HTML ( )   PDF(275KB)
    A pulse sequence of polarization transfer via long-range 1H-13C couplings is introduced. This technique has been carried out on a JEOL FX-90Q NMR spectrometer. It is demonstrated that the selective insensitive nuclei enhancement by polarization transfer via long-range 1H-13C couplings (SELINEPT) is a powerfull tool for measuring quaternary carbon atoms and assignment of the peaks in 13C spectra through determining some model compounds.
    13C-NMR STUDIES OF THE CARBONATION OF TOLUENE Ⅰ. Protonation of Toluene
    Wu Daxu
    Chinese Journal of Magnetic Resonance, 1989, 6(2): 255-260.  
    Abstract     HTML ( )   PDF(290KB)
    The 13C-NMR spectra of the toluene-alumium chloride-hydrogen chloride system were measured at room temperature. The fast chemical exchange between toluene and its protonated complex as will as complexes themselves in the solution has been verified by means of the 13C-NMR spectra, some anomalous phenomena in the experiments are interpreted in this paper.