The aim of this paper was to study the thermal degradation of soybean biodiesel attained by ethanolic route. The soybean biodiesel samples were subjected to heating treatment at 150 degrees C for 24 h in a closed oven under controlled atmosphere. During the experiments, samples were withdrawn at intervals of 3, 6, 9, 12, 15 and 24 h for physicochemical and thermophysical properties analysis. The biodiesel degradation was validated by Thermogravimetric analysis since their profiles for control and treated biodiesel were different. Also, H-1 NMR confirmed this result due to a significant reduction at the signals related to the 1H located near to the double bonds in the unsaturated ethyl esters in agreement with an iodine index reduction and viscosity increase observed during degradation. Nevertheless, degraded biodiesel, under study conditions, preserved its thermophysical properties. These results may be relevant to qualify the produced biodiesel quality and collect physicochemical and thermophysical data important for applications in combustion studies including project of fuel injection systems. (C) 2016 Published by Elsevier Ltd.