Atomic force microscopy (AFM) has been successfully used to study the activation energy for evaporation of pentaerythritol tetranitrate (PETN) nanoislands formed by spin coating. These islands are annealed isothermally in the temperature range of 30-70°C for a given time and are scanned with AFM in contact mode at room temperature. The volume of these islands does not change significantly up to about 35-40°C indicating that sublimation is not significant below 40°C. Above 40°C, the islands start shrinking, and the rate of weight loss is analyzed as a function of temperature. The activation energy of evaporation using AFM was found to be similar to that for bulk PETN crystals using thermogravimetric analysis (TGA) at higher temperatures (110-135°C). These results demonstrate that AFM is a useful tool to measure thermodynamic properties with a nanoscale probe.