A controlled heating experiment has been carried out on selected geological limestone samples obtained from the Yucatan peninsula to establish a heating temperature calibration curve for the determination of heating temperatures through Fourier Transform Infrared Spectroscopy (FTIR-ATR) ratios of υ2/υ4 peak intensities. This curve – the first produced in the Mayan area – will greatly benefit the study of the lime calcination technology employed by the ancient Maya society. This model was then applied to the study of an archaeological pit-kiln located on the northern Maya lowlands, allowing us to describe the temperature distribution at which the limestones were exposed within the structure, and consequently providing insights on the lime manufacturing process and the control of fire achieved by this culture.