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Poly(vinylpyrrolidone): Configurational assignments by one- and two-dimensional NMR spectroscopy
Authors:Kaushik Dutta  A. S. Brar
Abstract:The configurational assignment of poly(vinylpyrrolidone) (PVP) prepared by peroxide-initiated solution polymerization was studied by the combination of one- and two-dimensional NMR spectroscopy. The broad and overlapping 1H-NMR and 13C{1H}-NMR spectra of PVP were assigned to the configurational triad, pentad (CH, 2CH2, 3CH2, and 4CH2 regions), and tetrad (β-CH2 region) sequences. The configurational assignments of the various carbon resonances were confirmed with the help of two-dimensional experiments such as heteronuclear single quantum correlation (HSQC), heteronuclear single quantum correlation–total correlation spectroscopy (2-D HSQC–TOCSY). The various geminal and vicinal couplings within the configurational sequences were assigned with the help of total correlation spectroscopy (TOCSY low mixing time). The propagation pathway was studied using the 13C{1H}-NMR (carbonyl carbon) and 15N{1H}-NMR spectra. The 15N{1H} resonance signals were assigned to pentad-level configurational sequences. The results obtained by the analysis of the area under the resonance signals confirmed that poly(vinylpyrrolidone) obeys Bernoullian statistics. © 1999 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 37: 3922–3928, 1999
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