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An important step in the conservation of old paper documents is the analysis of both the medium and the ink, in an attempt first to determine the extent of deterioration and degradation and then to choose the best preservation and restoration solutions. Our paper focuses on the analysis of three old documents displayed at the ‘Poni-Cernătescu’ Museum in Iaşi City, Romania by optical microscopy (OM), scanning electron microscopy and energy dispersive X-ray spectroscopy (SEM-EDX), micro-FTIR spectroscopy and FT-Raman. Thus, the morphology and chemical composition of the paper media and the type of ink, as well as the cellulose crystallinity index were determined. PCA (Principal Component Analysis) was also used while relying on spectra collected by FTIR spectroscopy. We were able to determine the extent of degradation of the documents by corroborating all these findings.