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As a contribution to exploring non-destructive strategies for the evalua-tion of the state of degradation of paper documents, two SPME on-fiberderivatization methods were developed for the analysis of low molarmass carbonyl and carboxyl compounds formed during paper degrada-tion upon ageing. The two SPME methods involved the specific extrac-tion of carbonyl and carboxyl compounds using PFBHA and PDAM asderivatizing agents, respectively. They were first tested and validated inheadspace sampling mode where the emission from a groundwood pulppaper was characterized qualitatively and quantitatively. The methodswere then applied on a set of four papers of different composition anddegradation state obtained by artificial ageing. The second step wasaimed at extending the methodology for field application and involvedthe development of direct contact sampling of the VOCs emitted fromfour books of different composition, naturally aged, by inserting thederivatized SPME fibers inside the books core.The analyses are discussed in the light of the paper’s pulp compositionand their degradation state related to the artificial ageing. The resultsshowed that there was a close relation between the amount of VOCsemitted from paper and the composition of the paper, and that the gen-eral trend for both acids and aldehydes was an increase in the emissionswith ageing time, or occasionally, a plateau reached at the longest age-ing times. The VOCs emitted by the naturally aged books were consistentwith those of the artificially aged papers. Globally the emissions of alde-hydes were much lower than the emissions of acids and, for all thepapers the most abundant VOC was formic acid, both in the unaged andin the aged samples. This is noteworthy as formic acid has been recentlydesignated as highly aggressive towards cellulose.