A major impurity in poly (vinyl alcohol) (PVA) is sodium acetate which remains after its preparation by a base catalyzed hydrolysis of poly(vinyl acetate), and the amount of sodium acetate in commercial PVA samples may reach several percentages. To establish an optimal condition for the removal of sodium acetate, several washing parameters such as washing period, solvent polarity, and temperature were investigated in this study. Nuclear magnetic resonance (NMR) spectroscopy was successfully applied to determine the residual amounts of sodium acetate in the purified poly(vinyl alcohol). The relative integral value for the methyl peak of sodium acetate in PVA was converted to a relative mass value and finally to the sodium acetate content contained in PVA. The results showed that over 95% of sodium acetate in PVA was removed by a washing of PVA with distilled water within 2 h. When methanol was used as a washing solvent, a higher temperature than room temperature was required for an effective removal of sodium acetate. (c) 2007 Wiley Periodicals, Inc.