Sensitive determination of glycerol by derivatization using a HPLC-DAD method in biodiesel samples

• Published in: Analytical methods Vol. 7; no. 18; pp. 7805 - 7810
• Main Authors: Ahmed, Muhammad Arif, Khan, Ijaz, Hashim, Jamshed, Musharraf, Syed Ghulam
• Format: Journal Article
• Language: English
• Published: 01.01.2015
• Subjects: Arrays; Biodiesel; Byproducts; Chlorides; Copper chlorides; Diodes; Glycerols; Mathematical analysis; Transesterification
• ISSN: 1759-9660; 1759-9679
• DOI: 10.1039/C5AY01761K

Biodiesel is mainly produced through a transesterification reaction which yields biodiesel and glycerol, a by-product. This article describes the quantification of glycerol based on high performance liquid chromatography (HPLC) using a diode array detector (DAD) in various biodiesel samples through post-derivatization. Glycerol was converted into a UV active product i.e. glyceryl tribenzoate (GTB) through a simple and effective esterification reaction using benzoyl chloride and copper chloride as the catalyst under mild conditions. Optimized reaction conditions (affording a 90% yield) were obtained by using copper chloride (17 mol%), benzoyl chloride (12.0 equiv.) and triethyl amine (11.0 equiv.). The limit of detection and limit of quantification were found to be 0.23 μg mL −1 and 0.76 μg mL −1 , respectively. The developed and validated HPLC-DAD method is sensitive, selective, reproducible and successfully applied for the quantification of glycerol in biodiesel from various sources.