Several degree-epoxidized linseed oils (8, 20, 35, 40, 47 and 54%) were prepared for changing different reaction parameters such as temperature, amount of peroxide and enzyme of the well studied chemoenzymatic epoxidation method. The epoxidation reaction following was carried out by Infrared spectroscopy (FTIR) and Proton Nuclear Magnetic Resonance (H1NMR) which are the most usual spectroscopes for this propose. However, microRaman spectroscopy and Differential Scanning Calorimetry (DSC) characterization were used in this work as complementary techniques. Particularly, DSC permitted to correlate the epoxy-aperture energy to each epoxidation percentage making it another optional technique for quantify epoxidation levels in triglycerides.