Poly(1-oxodimethylene) was synthesized via oxidation of poly(vinyl alcohol) with a hydrogen peroxide/hydrobromic acid system. The content of the carbonyl groups in poly(1-oxodimethylene) depended on the amount of water added, and lower amounts of water were suitable for efficient oxidation due to higher acidity of the reaction system. The highest content of carbonyl groups was estimated to be above 88% by the titration with hydrazine that reacted with the carbonyl groups in poly(1-oxodimethylene). The obtained poly(1-oxodimethylene) complexed with Cu and Ni ions under basic conditions. (c) 2013 Wiley Periodicals, Inc. J. Polym. Sci., Part A: Polym. Chem. 2013, 51, 25982605