Gas generation from molding materials creates a complex atmosphere in the mold–metal interface and is one of the primary causes of defects in cast components. Moisture, crystalline water, and decomposing binders are significant gas sources. The presence of volatiles and decomposing binder in the mold also affects the rate of heat absorption from the solidifying metal during the casting process. This work presents a measurement methodology to evaluate the rate and volume of gases generated from sand mixtures in combination with the temperature distribution and applied thermal analysis. The presented results show high reproducibility of the method. The thermal analysis results provide the start and end temperature of the binder decomposition reactions and the corresponding heat absorbed in this interval. The results obtained from the presented methodology can be used to validate the models/simulation tools developed to predict the gas evolution and related transport phenomena in the sand casting process.