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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 8 Issue 1, 05 March 1991 Previous Issue   Next Issue
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    CIDNP STUDY ON THE PHOTOCHEMICAL REACTION OF BENZOIN AND DERIVATIVES
    Jang Hongjan, Yan Baozhen, Li Ercheng, Xu Guangzhi
    Chinese Journal of Magnetic Resonance, 1991, 8(1): 1-10.  
    Abstract     HTML ( )   PDF(476KB)
    Photochemical reactions of benzoin and its derivatives have been investigated by photo-CIDNP technique We could deduce that the photochemical reaction products of (a), (c) and (b), (d) were second recombination products by using free radical-trapping agent with different concentrations. We discussed the reason about the variation of reaction mechanisms of (e) and (f) that differed in substituting groups.
    THE STUDY OF 13C CHEMICAL SHIFT OF β-NAPHTHOFLAVONES AND β-NAPHTHOFLAVONONES
    Wang Dong, Lu Yixian, Gao Congyang, Cai Mengshen
    Chinese Journal of Magnetic Resonance, 1991, 8(1): 11-18.  
    Abstract     HTML ( )   PDF(439KB)
    13C chemical shifts of 14 kinds of β Naphthoflavoncs and β-Naphthoflavonones have been studied. The chemical shift changes of these compounds are almost identical with those of flavones. All carbon chemical shifts have been assigned on the basis of COSY, HETCOR, HETCOLOC and PBB, DEPT, QUAT experiments
    APPLICATION OF NOE AND 2D NMR SPECTROSCOPY TO THE ASSIGNMENT OF 1H AND 13C CHEMICAL SHIFTS IN SESQUI-TERPENOIDS
    Sang Hong, Wang Hanging, Tu Yongqiang
    Chinese Journal of Magnetic Resonance, 1991, 8(1): 19-28.  
    Abstract     HTML ( )   PDF(512KB)
    The stereochcmical and structural analysis of two sesquiterpenoids was carried out using nuclear magnetic resonance spectroscopy. Several methods, including 1H-1H two-dimensional shift correlation spectroscopy, 13C-1H two-dimensional shift correlation spectroscopy, COLOC (COrrelation spectroscopy via LOng range Coupling), DEPT (Distortionless Enhancement by Polarization Transfer) were used for chemical shift assignment and configurational analysis. Nuclear Overhauser Effect Spectroscopy was used to establish the stereochemistry. This investigation demonstrates the power of two-dimensional NMR techniques and the Nuclear Overhauser Effect (NOE) in the structural determination of natural products.
    ESR STUDY OF THE OXIDATION OF SOME ACIDIC PHOSPHATE (PHOSPHONATE) OXOVANADIUM COMPLEXES IN THF
    Chen Deyu, Huang Lingbo, Feng Yafei, Cheng Chaorong, Xu Yuanzhi
    Chinese Journal of Magnetic Resonance, 1991, 8(1): 29-37.  
    Abstract     HTML ( )   PDF(496KB)
    ESR method has been used to study the dynamics during oxidation process of some acidic phosphate (phosphonate) oxovanadium complexes in THF. The effects of temperature, concentration and nature of complexes on reaction rate and reaction reversibility have been examined. Dynamical parameters-reaction order, reaction rate constant and the activation energy of reaction were calculated.
    SELECTIVE LONG-RANGE DEPT AND 2D NMR STUDIES OF N-ETHYLSISOMICIN SULFATE
    Miao Zhenchun, Feng Rui, Miao Changcheng, Jiang Xunfeng
    Chinese Journal of Magnetic Resonance, 1991, 8(1): 39-44.  
    Abstract     HTML ( )   PDF(350KB)
    A new aminoglycoside antibiotic, N-ethylsisomicin, was obtained by synthesis from sisomicin. According to the selective long-range DEPT, 13C-1H COSY and 1H-1H COSY experiments,its structure has been elucidated as (1), and total assigment of 13C and 1H NMRspectra achieved.
    IMPROVEMENT OF RESOLUTION IN LPSVD SPECTRA WITH PROPORTIONAL EXPONENTIAL WEIGHTING
    Li Bin, Huang Yongren
    Chinese Journal of Magnetic Resonance, 1991, 8(1): 45-54.  
    Abstract     HTML ( )   PDF(562KB)
    In practice, LPSVD is one of the most interesting linear-prediction techniques instead of FFT now. In this paper, a method is proposed by means of proportional exponential weighting which is performed after LPSVD, one can keep all characteristic parameters in HRNMR-spectra and improve their resolution, so far as a spectrum can be reconstructed by a group of lines with the same chemical shifts, intensities or integration of FFT spectra.
    SUBSTITUENT CHEMICAL SHIFT (SCS) AND THE SEQUENCE STRUCTURE OF ETHYLENE-α-OLEFIN COPOLYMERS Ⅱ.Method of SUBSTITUENT Chemical Shift (SCS)
    Zhou Zinan, Tian Wenjing, Wu Shengrong, Zhang Jianguo, Pel Fengkui
    Chinese Journal of Magnetic Resonance, 1991, 8(1): 55-61.  
    Abstract     HTML ( )   PDF(437KB)
    A method, substituent chemical shift (SCS), which is used in assignments of the 13C NMR spectra of ethylene-α-olefine copolymers, is proposed in this paper. The SCS method reveals the corresponding relation bctwce the peaks of spectrum of the copolymer and its sequences. At the same time, the relation is elucidated in a systematic way. The 13C NMR spectra of the copolymers are firstly divided into two categories according to the above mentioned relation apparent or not. Secondly, three critcrions for classification are suggested:SCS parameters (S1 and S2), spectrum of comonomer homopolymer and electrowithdrawing or electrodonating of substituent. Finally, the SCS method is compared with the Grant-Paul method in many ways.
    THE APPLICATIONS OF NUCLEAR SPIN RELAXATION TO POLYMER DYNAMICS AND INTERMOLECULAR INTERACTIONS
    Yan Xin, Wang Dehua, Qian Baogong
    Chinese Journal of Magnetic Resonance, 1991, 8(1): 62-62.  
    Abstract     HTML ( )   PDF(87KB)
    The correlation functions of the side-groups and side-chains of polymers are obtained for nuclear spin relaxation if the segmental motion of the polymers is described by VJGM model, these functions are derived from unequal two-side and three-site jump internal rotation, diffusion internal rotation, restricted internal rotation and multiple internal rotation. The corresponding spectral density functions are also given, and these functions are used to interpret the nuclear spin relaxation data of the side-groups of some polymers. The average spectral density functions of side-groups are derived under the magic angle spinning, the correlation times and diffusion coefficients of the side-groups of crosslinked poly (methyl methacry-latcs) and solid poly(vinylbutyral) are obtained by using these average spectral density functions. The multiphase structures of nylon 6, poly (ethylenc glycol) and its complexes are investigated with cross-polarization and magic angle spinning techniques.
    Three methods using nuclear spin relaxation are presented for studying the intermolecular interaction between polymers and solvents:First, the molecule of tetrachloromethane is used as a "probe" to detect the intermolecular interaction between polymers and tetrachloromethane; Second, the contribution to the spin-lattice relaxation of the quaternary carbons due to the intcrmolecular dipolar interaction is used to calculate the poly (butyl methacrylate)-solvent interaction variables; Third, the intermolecular interaction variables are obtained from the intermolecular heteronuclcar crossrelaxation rates. The heteronuclear cross-relaxation rates are also used to determine the distances among heteromuclei, the general formula for Calculating distances is derived, the experimental results for polymers testify that the formula is correct.
    It can be shown with the two-dimensional heteronuclear Overhauser effect technique that the dipolar interaction between the quaternary carbons in polymers and their nearest protons dominates the spin-lattice relaxation of the quaternary carbons. The two-dimensional cadmium-113-proton Overhauser effect spectra of a few cadmium compounds are first reported.
    SUBSTITUENT CHEMICAL SHIFT (SCS) AND THE SEQUENCE STRUCTURE OF ETHYLENE-α-OLEFINE COPOLYMERS Ⅲ. Quantitative Analysis
    Zhou Zinan, Tian Wenjing, Wu Shengrong, Zhang Jianguo, Pei Fengkui
    Chinese Journal of Magnetic Resonance, 1991, 8(1): 63-72.  
    Abstract     HTML ( )   PDF(526KB)
    In analysis of sequence structure of ethylenc-α-olefine copolymers methylene (CH2) βγ and γδ which present the inverse units of comonomer in chain of the copolymer are assigned to VV dyad and EEV triad, respectively. At the same time, both CH2 δδ and δδ+ are assigned to EE dyad. But partition of intensity Iδ+δ+ characterizing long sequence of ethylene between EE dyad and EEE triad is a key task for treating the sequence distribution of the copolymer. In fact, intensity Iδ+δ+ should not be divided equally. In order to revise it deduction is performed by Bovey's relationship and Randall's statistical method of polymer sequence. Therefore, the exact representation, exact and approximate solution of revisionary value A are all obtained successfully. The approximate solution obtained under condition of regular chain is identical with Ray's result. When content of comonomer in copolymer is low, the partitions of Iδ+δ+ between EE and EEE is almost equal.
    In level of dyad and triad, there are 13 peaks altogether on the 13C NMR spectrum of ethylenc-α-olefine copolymer, where 10 peaks belong to CH2 and the other 3 to CH. A set of formula calculating sequence distribution could be proposed directly by using those intensities of peaks mentioned above. All information of copolymer sequence structure could be obtained undoubtedly based on it. Hence the method presented here is a satisfactory and universal for studying sequence structure of ethylene-α-olefine copolymers.
    THE PRINCIPLES OF NOVEL NMR METHOD FOR THE DETERMINATION OF ALKALINE EARTH METAL MIXTURES IN SOLUTIONS
    Fedorov L. A, Yuan Hanzhen, Zuo Maoli, Shen Lianfang
    Chinese Journal of Magnetic Resonance, 1991, 8(1): 73-80.  
    Abstract     HTML ( )   PDF(492KB)
    The conditions of forming complexes stable in the NMR time scale, for alkali-earth metals-strontium, barium and calcium were investigated. Most suitable ligand for forming such complexes-cryptand C222 was found 13C NMR spectra of akali-earth metal and alkali metal-sodium, potassium and lithium complexes in deuterochloroform were studied and interpreted. 13C NMR signals of free ligand and its complexes with alkali earth metals which should be used for analytical purposes were assigned. 13C NMR spectra of different mixtures of alkali-earth and alkali metals in chloroform were studied. It was shown that in the spectrum of a mixture of barium, calcium and strontium in concentration of 0.001M for each metal under excess amount of free ligand, individual signals corresponding to free ligand and each of the ions were observed. These signals could be integrated with sufficient accuracy and each characterizes concentration of one of the metal ions correspondingly. These observed for the first time results allow to develop, in principle, a new method of inorganic analysis by 13C NMR spectroscopy. Suggestions of analytical methods for the NMR-determination of alkali-earth metals in their mixture were discussed in detail. The method could be extended to the analysis of more complicated mixtures including alkali metal series. Spectra were run on Varian XL-200 spectrometer.
    CARBON-13 NMR SPECTRA OF COALS AT HIGH MAGNETIC FIELD+
    Hu Jianzhi, Ye Chaohui, Chen Deyu
    Chinese Journal of Magnetic Resonance, 1991, 8(1): 81-88.  
    Abstract     HTML ( )   PDF(481KB)
    The aromaticities (fa) of coals measured at high magnetic field via static 13C CP spectra are consistent with those measured at low field by means of high resolution 13C CPMAS. Therefore, the demand for fast sample spining was avoided while high NMR detective sensitivity was maintained at high field.
    NMR INVESTIGATION OF INTERACTION OF GLYC YL-L-LEUCINE WITH Ho (ClO43 AND Yb (ClO43 IN AQUEOUS SOLUTION
    Ren Jinan, Niu Chunji, Pei Fengkui, Wang Wenyun, Ni Jiazan
    Chinese Journal of Magnetic Resonance, 1991, 8(1): 89-98.  
    Abstract     HTML ( )   PDF(566KB)
    The interaction of Glycyl-L-leudne with trivalent paramagnetic lanthanide cations, Yb3+ and Ho3+, was studied by 13C NMR The lanthanide-induced shifts are separated into contact and dipolar components. It was found that the carbon atom adjacent to the carboxyl group experiences significant contact interaction and therefore the ytterbium-induced shifts cannot be directly used for the analysis of the peptide conformation at least in this case. In aqueous solution (pH 3.31) the peptide is coordinated to the lanthanide ions via its carboxyl group. The peptidc linkage and the amino group are not involved in the coordination. The peptide conformation is analysed from the values of the geometric factor and the results indicate that in the complex the segments C1-C2-C5-C6, C2-C5-C6-C8 and C2-N-C3-C4 arc in trans form while C2-C5-C6-C7 and C1-C2-N-C3 in gauch form.
    2D NMR SPECTROSCOPIC STUDIES OF FLAVONOID FROM OXYTROPIS GLABRA
    Yu Rongmin, Li Xian, Zhu Tingru, Yoshihiro Harigaya, Yaeko Konda, Masayuki Onda
    Chinese Journal of Magnetic Resonance, 1991, 8(1): 99-106.  
    Abstract     HTML ( )   PDF(417KB)
    A flavonoid glycoside has been isolated from Oxytropis glabra D C (Leguminosae). This flavonoid was identified to be 3-O-[α-L-rhamnopvranosyl (1-6)-β-D-glncopyranosyl]-kaempferol by 2D NMR[1H-1H and 1H-13C (one-bond and long-range) COSY] and other physical-chemical methods.
    1H GOLDMAN-SHEN EXPERIMENT ON CRYSTALLINE AND ADSORBED WATERS IN CaSO4·(1/2) H2O POWDER
    Li Gengying, Wu Xuewen
    Chinese Journal of Magnetic Resonance, 1991, 8(1): 107-112.  
    Abstract     HTML ( )   PDF(331KB)
    1H cross relaxation time between crystalline and adsorbed waters inCaSO4 1/2 H2O powder was found to be 55.1 ms by use of the Goldman-Shen pulse sequence. In experiment, it was discovered that the narrow component ofthe 1H spectrum line decays with three time constants. The present paper gives some explanations for the experimental results.
    A DEDICATED ETHERNET COMMUNICATION PROTOCOL-BRUKNET
    Hu Hongbin, Li Chao, Li Hong
    Chinese Journal of Magnetic Resonance, 1991, 8(1): 113-116.  
    Abstract     HTML ( )   PDF(216KB)
    A dedicated ethernet communication protocol-BRUKNET developed by Bruker corporation was introduced. It provides a high speed data communication between ASPECT 2000/3000 and other computers using the ethernet as transfer medium.
    APPLICATION OF PROTON-DETECTED LONG-RANGE 2D C-H CORRELATION
    Zhai Chun, Ruegger Heinz, Rodger Charles
    Chinese Journal of Magnetic Resonance, 1991, 8(1): 117-122.  
    Abstract     HTML ( )   PDF(351KB)
    In this paper we present the apphcation of proton-detected method to a natural product struturc elucidation and compare with the direct detection.
    A PRECISION MARGINAL OSCILLATOR-TYPE NQR SPECTROMETER AND IT'S APPLICATION
    Fang Dehui, Liu Dehai, Zheng Xiaoli, Zhang Bide
    Chinese Journal of Magnetic Resonance, 1991, 8(1): 123-130.  
    Abstract     HTML ( )   PDF(1180KB)
    A precision marginal oscillator-type nuclear quadrupole resonance (NQR) spectrometer using field effect transistors (JFET'S) is described in this paper. The frequency is succesivcly adjustable by several ranges from 14 MHz to 35 MHz, This spectrometer shows a high sensitivity and small wave shape distortion. At room temperature, the measuring accuracy of NQR frequency of 35Cl in polycrystallinc powder of potassium chlorate sample is about 3×10-6, the signal to noise ratio (S/N) of NQR spectrum of 35Cl in recrystallized sample is greater Than 150. The obtained chlorine's quadrupolc coupling ratio (eQq) 35Cl/(eQq) 37Cl in potassium chlorate, sodium chlorate and sodium chloride art 1.2687363, 1.2687306 and 1.2687661 respectively. The relation of nuclear quadrupole resonance frequency and temperature have been studied by 35Cl in polycrystalline powder sample when the temperature was varied from 77 K to 393 K.