Three kinds of acrylonitrile - styrene (AN - ST) copolymers with different molar ratios were preparedand reacted with superoxide anion (O
2_??_) generated from electr o-chemical reduction of O
2_??_ and KO
2 in dimethylformamide (DMF) solution at 40°C under nitrogen atmosphere. Molecular weight of the polymers decreased with increase in O
2 concentration. IR and UV spectroscopies indicated the formation of hydr oxyl, carbonyl, α, β- unsaturated carbonyl, and polyene structures. These change s are largely dependent on the AN composition in the polymers and O
2_??_ concentration. Similar results were observed in both reaction systems of electrochemically generated O
2_??_ and KO
2. The reaction mechanisms were discussed on the basis of the obtained results.
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