%0 Journal Article %1 Ando2001a %A Ando, Shinji %A Harris, Robin K %A Holstein, Peter %A Reinsberg, Stefan A %A Yamauchi, Kazuo %D 2001 %J Polymer (Guildf). %K %N 19 %P 8137--8151 %R 10.1016/S0032-3861(01)00303-2 %T Solid-state1H-static,1H-MAS, and1H →19F/19F →1H CP/MAS NMR study of poly(vinyl fluoride) %V 42 %X Solid-state1H →19F-CP/MAS,19F →1H CP/MAS, and1H fast MAS NMR spectra have been investigated for a semicrystalline polymer, namely poly(vinyl fluoride) (PVF), together with its solution-state19F spectrum and static solid-state1H pulsed and broad line NMR measurements. The static1H pulsed NMR measurements of T1pHand T2Hshowed the two-phase (immobile and mobile) nature, and the Goldman-Shen type phase selection at 130°C indicated that a measure for the lamellar size yields about 4.2 nm. Although the solid-state19F-CP/MAS spectrum shows a featureless lineshape, the mobile region was selectively observed by a newly developed DIVAM pulse sequence. Solid-state spin-lock experiments showed significant differences in T1pFand T1pHbetween the immobile and mobile regions, and the effective time constants, THFand T1pwhich were estimated from the1H →19F CP curves, also clarify the difference in the strengths of dipolar interactions. Furthermore, the1H →19F inversion recovery CP (IRCP) experiment was more advantageous in observing the relatively weak dipolar interactions in the mobile region. The inverse19F →1H CP/MAS and1H →19F CP-drain MAS experiments gave complementary information to the1H →19F CP/MAS spectra, although spinning at 35 kHz is necessary to separate the signals between CHF and CH2protons in the1H spectra. The hetero-nuclear dipolar oscillation behaviours and the effective time constants, THF, TFH, and T1pdetermined from the1H →19F CP/MAS, CP-drain MAS, and19F →1H CP/MAS experiments are consistent with each other. In addition, the value of NF/NH(N is a spin density) estimated from the CP-drain curve is equivalent to that calculated from the chemical structure. © 2001 Elsevier Science Ltd.

@article{Ando2001a, abstract = {Solid-state1H →19F-CP/MAS,19F →1H CP/MAS, and1H fast MAS NMR spectra have been investigated for a semicrystalline polymer, namely poly(vinyl fluoride) (PVF), together with its solution-state19F spectrum and static solid-state1H pulsed and broad line NMR measurements. The static1H pulsed NMR measurements of T1pHand T2Hshowed the two-phase (immobile and mobile) nature, and the Goldman-Shen type phase selection at 130°C indicated that a measure for the lamellar size yields about 4.2 nm. Although the solid-state19F-CP/MAS spectrum shows a featureless lineshape, the mobile region was selectively observed by a newly developed DIVAM pulse sequence. Solid-state spin-lock experiments showed significant differences in T1pFand T1pHbetween the immobile and mobile regions, and the effective time constants, THFand T1pwhich were estimated from the1H →19F CP curves, also clarify the difference in the strengths of dipolar interactions. Furthermore, the1H →19F inversion recovery CP (IRCP) experiment was more advantageous in observing the relatively weak dipolar interactions in the mobile region. The inverse19F →1H CP/MAS and1H →19F CP-drain MAS experiments gave complementary information to the1H →19F CP/MAS spectra, although spinning at 35 kHz is necessary to separate the signals between CHF and CH2protons in the1H spectra. The hetero-nuclear dipolar oscillation behaviours and the effective time constants, THF, TFH, and T1pdetermined from the1H →19F CP/MAS, CP-drain MAS, and19F →1H CP/MAS experiments are consistent with each other. In addition, the value of NF/NH(N is a spin density) estimated from the CP-drain curve is equivalent to that calculated from the chemical structure. {\textcopyright} 2001 Elsevier Science Ltd.}, added-at = {2023-12-13T01:52:23.000+0100}, author = {Ando, Shinji and Harris, Robin K and Holstein, Peter and Reinsberg, Stefan A and Yamauchi, Kazuo}, biburl = {https://www.bibsonomy.org/bibtex/2d114faf07a52467b3e7f42234d8dbff5/admin}, doi = {10.1016/S0032-3861(01)00303-2}, interhash = {77a5e6cce9ea4d16bc3df63caf1c60d0}, intrahash = {d114faf07a52467b3e7f42234d8dbff5}, issn = {00323861}, journal = {Polymer (Guildf).}, keywords = {}, number = 19, pages = {8137--8151}, timestamp = {2023-12-13T01:52:23.000+0100}, title = {{Solid-state1H-static,1H-MAS, and1H →19F/19F →1H CP/MAS NMR study of poly(vinyl fluoride)}}, volume = 42, year = 2001 }