The spectral assignment of poly(vinyl alcohol) (PVA) prepared by the basic hydrolysis of poly(vinyl acetate) was studied using a combination of one and two-dimensional NMR spectroscopy. The ~(13)C{~1H} and ~1H NMR spectra of the homopolymer (PVA) were assigned to the configurational pentads (CH region) and tetrads (CH_2 region). These assignments were substantiated by the use of two dimensional heteronuclear single quantum correlation (HSQC), heteronuclear single quantum correlation - total correlation spectroscopy (HSQC-TOCSY) and total correlated spectroscopy (TOCSY) experiments.
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