AbstractThe formation of vanillin and syringaldehyde during an oxygen delignification process was evaluated. The cleavage of conjugated Cα-Cβ bonds in phenolic lignin caused by the attack of oxygen leads to the formation of aromatic aldehydes and ketones. The formation mechanism was confirmed by the organic compounds identified in the spent liquor by GC/MS. Additionally, the formation of aromatic aldehydes and ketones of hardwood, softwood, and grass was investigated. The results showed that the formed aromatic aldehydes and ketones were related to the units of lignin structure. Among the aromatic aldehydes and ketones present in the spent liquor from oxygen delignification, vanillin and syringaldehyde are of high content, making the spent liquor a potential resource for vanillin and syringaldehyde production.