Two different pulse calibration techniques to estimate the total quantities of evolved gaseous substances formed in thermogravimetric (TG)-FTIR runs were compared and assessed. A gas-pulse calibration method was based on the use of a specific device able of sending a known quantity of a gaseous compound of interest to the FTIR analyzer. A second calibration method was based on the vaporization in the TG analyzer of liquid solutions of the compound of interest. Data obtained by these techniques were compared to those from conventional concentration-based calibration. The results confirmed the reliability of pulse calibration techniques to obtain quantitative data on evolved gaseous products in TG-FTIR applications. Moreover, both the gas-pulse and the vaporization-based calibration techniques proved to have several advantages with respect to conventional techniques. Among these are the need of a more limited number of standards and no need for online gas dilution systems.