Ultrasonic extraction of oil shale bitumen and study of its structural features using GC-MS and NMR techniques

Abstract

ABSTRACT Oil shale is a raw material that is considered to be an alternative fossil fuels and it is widely used in producing energy and chemicals. Oil shale bitumen identification are not widely described in literature. This article tackles the structural elucidation of oil shale bitumen using gas chromatography-mass spectrometry (GC-MS) and nuclear magnetic resonance (NMR) spectroscopy with a short sample preparation step, based on ultrasonic-assisted liquid extraction. The ultrasonic-assisted extraction was examined in terms of solvent type and volume, sample size, sonication time and temperatures. A bitumen recovery of 17.7 wt% dmmf (dry-mineral-matter-free) was achieved when 0.50 g of shale was mixed with 20 mL THF and sonicated for 10 min at ultrasonic power of 120 W at 45°C. GC-MS of the bitumen showed high polar oxygenated compounds with more than 20 wt% being esters and ethers. Small concentrations of thiols and amides have been also found. The structural identification of bitumen was carried out using 1H-NMR and 13C-NMR and the results showed highly aliphatic character bitumen, consisting of aromatic, paraffinic, naphthenic and olefinic hydrogen and carbon atoms. These results suggested that ultrasonic solvent extraction could be an efficient and environment-friendly method for obtaining of bitumen from oil shale.