Identification of Sulfur‐Containing Impurities in Biodiesel Produced From Brown Grease

Abstract

AbstractFatty acid methyl esters (FAME) from waste grease usually contain higher concentrations of sulfur (S) than allowed to meet the specified quality standard for biodiesel (<15 ppm). Brown grease lipid‐derived FAME was produced and fractionated by two passes through a wiped‐film evaporator (WFE) to produce three fractions: (1) a 120 °C pass distillate, (2) a 170 °C pass distillate, and (3) a heavy residue. Solid phase extraction (SPE) was used to concentrate the S species from the distillate fractions so that they could be detected by a gas chromatography–pulsed flame photometric detector (GC–PFPD) and GC–mass spectrometry (MS). The ethyl acetate and methanol (MeOH) fractions obtained by SPE of the 120 °C WFE distillate and methyl tert‐butyl ether and acetone fractions obtained by SPE of the 170 °C WFE distillate had the highest concentration of S and were, therefore, the best candidates for GC–PFPD analysis. GC–PFPD methods were developed to separate the S species adequately enough for those peaks to be analyzed by GC–MS which matched fragmentation patterns identified by the MS chemical library as tetrahydrothiophenes, dithiolanes, and thiophenes. MS fragmentation patterns were used to identify other, larger, S‐bearing species as sulfides and disulfides cross‐linking between two FAME molecules. The results obtained from this study provide a foundation for developing effective purification methods to remove S‐containing impurities from waste grease‐derived biodiesel.