In this work, we compared three methods of analysis of cellulose in paper subjected to accelerated ageing: size exclusion chromatography in combination with multiangle light scattering (SEC-MALS) detection, size exclusion chromatography in combination with diode-array detector and calibration using polystyrene standards (SEC-DAD), and asymmetric flow field–flow fractionation in combination with multiangle light scattering (A4F-MALS). Prior to separation, cellulose sample were derivatized with phenyl isocyanate to CTC and dissolved in tetrahydrofuran.