Intercalated materials containing iron and carbonate species were synthesized in this work to study their hydrolysis and condensation from sol to gel transition. The former material was designated as PV (perovskite) and the latter HT (hydrotalcite). Another sample containing neither of the indicated ions was designated as AlMg(OH)5 (aluminum magnesium hydroxide). The conversion energy of these materials for the hydrolysis and condensation reaction during the transition was estimated to be ≈14 cal/mol, much lower than the hydration energy of 10–14 kcal/mol computed using molecular dynamic simulation from the previous work. The energy consumed was interpreted as equivalent to the drop of temperature due to the endothermic reaction. PV material exhibited the highest swelling ratio, amounting to 76% from its dried weight, demonstrating its ability to intercalate water readily. HT sample, on the other hand, was completely saturated and did not dilate.