1260Infinity分析型SFC系统与蒸发光散射检测器快速筛查.PDFVIP

Fast screening of impurities in biodiesel using the Agilent 1260 In?nity Analytical SFC System in combination with evaporative light scattering detection Application Note Petrochemical Authors mV 160 1 P PPP PP 120 80 Maria Rambla-Alegre, Melissa 40 Glycerol 0 N. Dunkle, Frank David, Pat Sandra mV 0 250 2 1 2 34 OOO 5 min 200 Research Institute for Chromatography 150 and OO O Kennedypark 26 100 50 0 Glycerol 0 1 2 3 4 5 min B-8500 Kortrijk, Belgium Martin Vollmer Agilent Technologies, Inc. Waldbronn, Germany Abstract According to EU regulation, the concentration of residual glycerol, mono-, di- and triglycerides in biodiesel should be monitored. This analysis is normally performed by gas chromatography after derivatization of the sample. Alternatively, supercritical ?uid chromatography coupled to evaporative light scattering detection (SFC-ELSD) can be applied, eliminating the need for derivatization. Using the Agilent 1260 In?nity Analytical SFC System, excellent separation repeatability and good sensitivity were obtained, while the analysis time is approximately 6 minutes. The described SFC-ELSD method can be used for screening control of biodiesel (B100) samples. Introduction The interest in biodiesel is growing tremendously. Biodiesel is typically obtained from vegetable oils such as rape seed oil, sun?ower oil, soybean oil, or palm oil, by transesteri?cation, resulting in a mixture of fatty acid methyl esters (typically referred to as B100). According to EN Norm 14214, biodiesel samples should comply with a number of criteria 1. The EU Norm EN-14105 regulates the maximum residue level of monoglycerides (MG), diglycerides (DG), triglyceride (TG), and glycerol (Gly) in biodiesel. These maximum residue level ranges are 0.8% (w/w) for monoglycerides, 0.2% (w/w) for diglycerides and triglycerides, and 0.02% (w/w) for glycerol. The of?cial method to determine these residues involves derivatization by silylation (MSTFA) followed by the analysis of the silylated sample