The calcium silicate hydrate gel (C-S-H) was synthesized by the double decomposition method because of the simplicity and the quickness of the procedure. The structure of the C-S-H gels after 1 week and 4 weeks in contact with the formation solution was studied through Micro-Raman, Fourier Transformed Infrared Spectroscopy and 29 Si Nuclear Magnetic Resonance. Simultaneous thermodifferential-thermogravimetric analysis and mass spectrometry (DTA/TG/MS) was used to identify the amount of calcium carbonate formed due to the reaction between the calcium and atmospheric CO 2. With DTA/TG/MS, mass loss due to CO 2 was observed to take place at temperatures below 400ºC, unidentified to date, which might be associated with the CO 2 adsorbed on the C-S-H gel. Thus, in the TG analysis in the 300-430ºC range, both the loss of water due to the decomposition of the amorphous calcium carbonate (ACC) and the loss of CO 2 adsorbed on the gel must be considered. Additionally, polymerization of the gel and a decrease in the Ca/Si ratio was observed from the samples from 1 to 4 weeks.