Hydrogen peroxide (H 2 O 2 ) entrapment in silica hydrogels has potential to be used in various industrially important applications to increase H 2 O 2 stability. In this study, optimum conditions for hydrogel formation and H 2 O 2 stability were determined by varying the sodium content and initial H 2 O 2 concentration. Higher retention and better stability of H 2 O 2 were achieved with hydrogels at room temperature at low sodium concentration. Retention values of 89% were obtained with initial H 2 O 2 concentrations up to 10 wt %. H 2 O 2 decomposition in hydrogels followed a first-order reaction. Hydrogels were characterized by measuring their surface area, pore size, and pore size distribution by Brunauer−Emmett−Teller analysis and scanning electron microscopy. Mesoporous (3−24 nm) hydrogels with high surface area (1000−1400 m 2 /g) were obtained. In addition, the melting point of the entrapped H 2 O 2 -water mixture in the hydrogels was studied by low temperature differential scanning calorimetry.