Abstract: A process for the preparation of acrylic acid or methacrylic acid which comprises catalytically decomposing or converting in the presence of selenium the peroxide (peroxy) compounds formed during autoxidation or contained in the oxidate solution derived from the autoxidation of the respective acrolein or methacrolein, particularly, the conversion of permethacrylic acid and methacrolein monopermethacrylate to methacrylic acid.