In the present study, epoxidation and ozonolysis led to a decrease of 40.8 and 51.9 % in the degree of unsaturation of corn oil, respectively. Both products were initially characterized by Fourier transform infrared spectroscopy and 1H- and 13C-nuclear magnetic resonance spectroscopies. The heteronuclear single-quantum correlation spectroscopy (HSQC) analysis of the polyol obtained by epoxidation showed that carbinol hydrogen signals, located between 3.65 and 3.47 ppm, were correlated to carbon signals between 74.4 and 71.7 ppm. HSQC analysis of the polyol obtained by ozonolysis revealed these same chemical shifts at 3.64 and 62.9 ppm, respectively. Compared to pure corn oil, the differential scanning calorimetry of both corn oil-based polyols displayed the absence of any detectable melting peaks. However, the epoxidized derivative had a higher thermal stability than the ozonated sample, as shown by thermogravimetric analysis.