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Initiating depolymerization at ambient temperature by nonthermal air plasma provides a novel and promising route to convert polymer wastes to valuable small molecules. This study showed that the selectivity of partial oxidation of polyvinyl alcohol (PVA) initiated by nonthermal air plasma can be controlled by the polymer to TiO2 ratio and AC (alternative current) voltage and frequency. Transient responses to applying AC (alternating current) power showed that the CO2 led to the formation of CO, propionaldehyde, and acetaldehyde. Significant formation of propionaldehyde showed that -C-OH in PVA can be directly converted to CH3 in propionaldehyde, unraveling a new reaction pathway in nonthermal plasma chemistry. The selectivity of aldehydes is at the same level as that of CO2. The selectivity of aldehydes was further enhanced by nitrogen plasma while the selectivity toward CO2 was increased in the presence of TiO2. This study demonstrated that ambient nonthermal air plasma could provide a potentially effective approach for the selective conversion of polymers to desired small molecules.