Two series of gels were prepared by hydrolyzing TEOS with HCl or NH4OH catalyst. In the first series, the molar ratio of water to TEOS was 4:1 and the catalyst addition was (1 × 10−3), (4 × 10−3), (1 × 10−2), (4 × 10−2), and (1 × 10−1). In the second series, the catalyst addition was (1 × 10−3) moles and the molar ratio of water to TEOS was 2:1, 4:1, 8:1, 16:1, and 32:1. Dried samples were characterized for surface area, porosity and C and H content. Samples were heated to 800°C and thermogravimetric weight loss was recorded. Both HCl and NH4OH are catalysts for hydrolysis, but during polymerization, the relative rates of hydrolysis and condensation determine resulting dried microstructures.