Biodiesel is defined as the monoalkyl ester derivative of long-chain fatty acids, originated from renewablesources, such as vegetable oils or animal fats. The most common use of biodiesel is direct substitution offossil fuels in compression-ignition engines. The heating of vegetable oils can cause complementarydecomposition reactions, in which the results can also lead to the formation of polymeric compounds. Thiswork has been carried out to study the degradation process of biodiesel in different temperatures and exposuretimes. The degradation process of biodiesel affected its thermogravimetric and calorimetric profiles, indicatingthe formation of intermediary compounds. The spectroscopic data of degraded biodiesel suggested oxidativepolymerization, confirming thermal data. In the degraded biodiesel at 210
C for 48 h, the formation of gumoccurred, indicating that oxidative polymerization was completed.