Solid-state variable-temperature 1H MAS NMR studies on deuterated polyethylene.

作者: Q. Chen , H. Hurosu , I. Ando , X. Wu

DOI: 10.1016/S0926-2040(96)01254-4

关键词: Analytical chemistryMagic angle spinningProtonDeuteriumDecoupling (electronics)PolyethyleneDeuterium NMRProton NMRSolid-state nuclear magnetic resonanceChemistry

摘要: Abstract Solid-state varible-temperature/magic angle spinning(VT/MAS) 1 H NMR measurements were carried out on deuterated polyethylene. From these experimental results it was found that the chemical shift induced by conformational and morphological changes of polyethylene sample is within linewidth ≈ 0.5 ppm. Furthermore, from MAS/dipolar decoupling experiments resonance frequency proton varies linearly with inverse square deuterium power. This finding discussed theoretically.

参考文章(16)
C. A. Fyfe, J. R. Lyerla, W. Volksen, C. S. Yannoni, High-Resolution Carbon-13 Nuclear Magnetic Resonance Studies of Polymers in the Solid State. Aromatic Polyesters Macromolecules. ,vol. 12, pp. 757- 761 ,(1979) , 10.1021/MA60070A044
Richard Eckman, High resolution proton NMR of dilute spins in solids Journal of Chemical Physics. ,vol. 76, pp. 2767- 2768 ,(1982) , 10.1063/1.443229
Qun Chen, Takeyoshi Yamada, Hiromichi Kurosu, Isao Ando, Takeshi Shiono, Yoshiharu Doi, Structural characterization of solution-crystallized 13C-labeled polyethylene over a wide range of temperatures by means of high-resolution 13C NMR spectroscopy Journal of Molecular Structure. ,vol. 263, pp. 319- 327 ,(1991) , 10.1016/0022-2860(91)80074-E
A. Pines, S. Vega, M. Mehring, NMR double-quantum spin decoupling in solids Physical Review B. ,vol. 18, pp. 112- 125 ,(1978) , 10.1103/PHYSREVB.18.112
A. Pines, D. J. Ruben, S. Vega, M. Mehring, NEW APPROACH TO HIGH RESOLUTION PROTON NMR IN SOLIDS: DEUTERIUM SPIN-DECOUPLING BY MULTIPLE-QUANTUM TRANSITIONS Physical Review Letters. ,vol. 36, pp. 110- 113 ,(1976) , 10.1103/PHYSREVLETT.36.110
J. J. Dechter, R. A. Komoroski, D. E. Axelson, L. Mandelkern, Carbon‐13 NMR linewidths of polyethylenes and related polymers Journal of Polymer Science Part B. ,vol. 19, pp. 631- 651 ,(1981) , 10.1002/POL.1981.180190407
M. Takenaka, T. Yamanobe, T. Komoto, I. Ando, H. Sato, 13C.N.M.R. chemical shift and crystal structures of cyclic paraffins of long chain lengths Solid State Communications. ,vol. 61, pp. 563- 565 ,(1987) , 10.1016/0038-1098(87)90170-0
Leo Mandelkern, Crystallization of polymers ,(2002)