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MOLECULAR STRUCTURE OF CHAIN-EXTENDED MONOMERS AND MONO-DISPERSE OLIGOMERS FOR POLY(ARYL ETHER KETONE)S BY 13 C NMR AND CALCULATION
Ke Yangchuan, Hua Shiyin, Zhen Yubin, Zhaug Shanju, Wu Zhongwen
Chinese Journal of Magnetic Resonance, 1996, 13(3): 219-230.
To Characterize the molecular structure of oligomers and polymers of Poly(aryl ether ketone)s family,this paper presents a series of Chain-extended monomers and mono-dispersed Oligomers.The comparison researches on these compounds dissolved in DMSO-d6 (or DMSO-d6 +CDCl3 ) and H2 SO4 -d2 (or H2 SO4 ) are made by 13 C NMR method.Results show that, in H2 SO4 , their molecular structures are greatly polarized.Results from quantum mechanical calculation and dynamic 13 C NMR show that this polarization results from the charge unlocalization of bridge-bonds and aryl-rings in molecular chain induced by sulfo-group of H2 SO4 ,but not from the reaction of sulfo-group.The Polarization route for the titled compounds are firstly suggested.
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IN VIVO 19 F NMR STUDY ON METABOLISM OF 5-FLUOROURACIL IN MURINE LIVER AND IMPLANTED TUMOR
Yan Xianzhong, Li Hua, Du Zehan, Ruan Jinxiu
Chinese Journal of Magnetic Resonance, 1996, 13(3): 239-244.
Metabolism of 5-fluorouracil(5FU) in mouse liver and implanted S180 tumor was studied using in vivo 19 F NMR spectroscopy. The half-life of 5FU elimination is about 15-20min in liver and 50-60min in tumor.Catabolites of 5FU,fluorouredopropanic acid and α -fluoro-β -analine,were observed in livel, while only the fluoronucleotides,anabolites of 5FU,were observed in tumor. The results show that NMR spectroscopy is a powerful method for metabolic and pharmacokinetic studies.
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ASSIGNMENIS OF THE 1 H NMR AND 13 C NMR SPECTRA OF 9-FLUORENYLMALONOMTRILE AND ITS ANALOGUES
Zhu Xiaoqing, Yang Li, Guo Oingxiang, Wu Longmin, Liu Youcheng
Chinese Journal of Magnetic Resonance, 1996, 13(3): 245-252.
The 1 H NMR and 13 C NMR spectra of 9-fluorenylmalononitrile,ethyl α -cyano-α -(9-fluorenyl) acetate,α -cyano-α -(9-fluorenyl) acetamide have been reported and all the chemical shifts of 13 C and proton have been assigned according to substituent effeCt,H-H COSY,C-H COSY HMBC,MS spectra of their 9-deuterated compounds.
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ESR STUDY OF THE NATURAL DIAMONDS AND THE DIAMOND-LIKE MATERIALS
Zhou Jianwei, Yang Baolian, Hu Hongbing, Li Liyun, Qiu Jiangqing, Zeng Fanming, Guo Jiugao, Zhan Rujuan, Chen Feng, Ye Chaohui
Chinese Journal of Magnetic Resonance, 1996, 13(3): 267-275.
Five single crystals of the natural diamonds,four Synthetic diamonds and two diamond-like films (PCVD film) have been investigated by means of ESR method. The results show that there are four kinds of N-center free radicals and one kind of C-center free radical in the Ib type natural diamonds, and the unpaired electron is located on an antibonding orbital of the N3 impurity center in the IaB3 type natural diamonds.The ESR spectra of the Ib type synthetic diamonds are similar to the natural diamonds,except that the linewidthes are broader since they contain some paramagnetic elements,such as Ni,Fe,etc.For diamond films,the concentration of the C-center free radicals varies greatly. however,the concentration of the N-center free radicals,which are usually quite low in diamond-like films, varies relative slightly.Finally,the two satellite peaks of the C-center free radicals are found to be the direct evidence of the existence of hydrogen atoms in the PCVD films.
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STUDY ON ESR AND STRUCTURE PHASE TRANSFORMATION IN ZnS:Ag
Hou Bihui, Sui Yunxia, Han Shiyin, Li Bilin, Guo Changxin
Chinese Journal of Magnetic Resonance, 1996, 13(3): 277-282.
It was found with electron-spin-resonance(ESR) that the doped silver is Ag+ ,and no ESR signal or Ag2+ was observed in ZnS crystallite. With ESR of probe ion Mn2+ and X-ray diffraction analysis, it was found that a structure phase transformation from cubic lattice(β phase) to hexagonal(α phase) in ZnS crystallite is affectd by doped amount of Ag+ ion and calcination temperature. There is a reverse transformation phenomenon when Ag+ doped amount is 5×10-4 g/g and at 1100℃-1200℃.The Landé factor g of α phase is 2.006,the hyperfine constant a is 6.76mT,the g of β is 2.002,a is 6.81 mT from ESR of the Mn2+ .
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STUDIES ON 13 C NMR SPECTRA OF TRIS(2-METHYL-2-PHENYL PROPYL) TIN ARYLOXYACETATES
He Qinglin, Bao Ming, Tian Zuolin, Liu Baodian
Chinese Journal of Magnetic Resonance, 1996, 13(3): 300-302.
The
13 C NMR spectra of fifteen new tris(2-methyl-2-phenyl propyl) tin aryloxyacetates were recorded.The chemical shifts of various carbon resonances have been assigned on the basis of calculation and comparison with the chemical shifts of the model compounds.The data of the effect of substituent of
on the
13 C chemical shifts in benzene ring were obtained:C
ispo =30.0,C
ortho =-13.8,C
meta =0.8,C
para =-7.5.