Hydrogels of carboxymethylcellulose (CMC) with 2.5%, 25%, 50%, and 100% cross-linking were prepared. Cross-linking and stoichiometry was controlled by appropriate addition of CMPJ and determined by potentiometric titration. The cross-linked polymer was then sulfated using a sulfur trioxide-pyridine complex (SO3-Py) in a heterogeneous mixture. Water uptake of the gels was studied in relation to cross-linking, pH, and sulfation. FT-IR spectra of the gels were recorded at different pHs to evidence the hydrogen bonds. Hydrogen bonds formation between the chains may explain the correlation found between water uptake properties and the chemical composition of the gels.