H-1 nuclear magnetic resonance (n.m.r.) studies of two examples of poly(vinyl alcohol/vinyl acetate) copolymers, of differing residual acetate content and hydroxyl block size distribution, but similar acetate block size distribution, are reported. The studies were undertaken over the temperature range of 2 to 30-degrees-C, at 2-degrees-C intervals, in D2O solution. The data appear to show correlation with previously determined conformational changes in the polymer as a function of temperature; additionally the data suggest that differences in the composition of the copolymers are reflected in differences in their n.m.r. spectra.