Grains like barley and rye contain oil with a high amount of unsaturated fatty acids. The oil is the most sensitive grain component with regard to oxidation, that in turn limits the shelf life and sensory characteristics of roasted products [1]. Differential Scanning Calorimetry (DSC) is a nonchemical technique to determine oil quality parameters e.g. its oxidative stability [2]. The aim of current study was to assess the influence of roasting process on oxidative stability of oil extracted from barley and rye grains using combined data from Pressure Differential Scanning Calorimetry (PDSC), Gas Chromatography (GC) and Fourier-Transformed Infrared Spectroscopy in the middle range (MID-FT-IR). Roasting was conducted in a laboratory convective dryer, Memmert UFP400. Mentioned measurements were conducted for both fresh and roasted grain samples. PDSC experiments were carried out using a DSC Q20 TA Instruments, coupled with a high-pressure cell. Studied samples were placed in the platinum pan filled with oxygen, and pressurized in isobaric module (1400 kPa) in constant temperature of 120°C. PDSC curves registered were used to determine induction time. The determination of fatty acid composition was carried out by GC separation of fatty acid methyl esters formed from fatty acids naturally contained in studied oils. Infrared spectra were registered for every sample in the classic range of 4000–400 cm-1 with 1 cm−1 resolution, using System 2000 Perkin Elmer instrument. The Grams AI 8.0 and TQ Analyst 8 software were used for spectral data processing, statistical modelling hence oils evaluation. Single drop of studied samples with approximate volume of 0.5 cm-3 was placed on a KRS plate and covered by another KRS plate to form a film. Registration of 10 spectra for each sample with 20 scans for every spectrum was followed by spectra averaging and processing of the averaged spectrum. The analysis of data registered shows that roasting process has influenced the oxidation induction time, hence oxidative stability of studied oils. It was also observed, that spectral data from selected only ranges correlate with the induction time with statistical significance.