Wide range of rapid analytical methods intended for the physicochemical analysis of organic compounds are being actively developed. The present paper highlights the possibility of studying microquantities of polymer materials using a chip calorimetry (nanocalorimetry) method combined with atomic force microscopy (AFM). An experimental setup is presented for conducting combined studies using ultrafast chip calorimetry and AFM. The main technological aspects of combining the two methods are considered, and behavior of a nanocalorimetric sensor when interacting with a cold AFM cantilever for measurements of microquantities of polymer materials at different temperatures is addressed in situ.