1H NMR assisted quantification of glycerol carbonate in the mixture of glycerol and glycerol carbonate

Talanta. 2018 Feb 1:178:1001-1005. doi: 10.1016/j.talanta.2017.08.103. Epub 2017 Sep 1.

Abstract

Glycerol carbonate (GLC) is a very important chemical having a variety of application viz., green solvent in organic synthesis, an electrolyte in lithium batteries, wetting agent in cosmetics and precursor in polymer and food industry for the synthesis of 1,3-sn-diglycerides. Hence, it is vital to find out the quick and simple method for the quantification of GLC when it is synthesized via dimethyl carbonate (DMC) assisted transesterification with glycerol (GL). Present study, proposes simple, accurate and non destructive quantitative proton nuclear magnetic resonance (qHNMR) method for the determination of GLC. Based upon the study, two different equations are proposed to calculate the GLC employing the data obtained from the 1H NMR spectra. qHNMR results were also validated by preparing the standard mixtures of varying concentrations of GL and GLC. Further, to conform the developed method for a real application, GLC concentration was also estimated during CaO catalyzed DMC transesterification with GL. The qHNMR assisted GLC quantification were found consistent with those obtained from high-performance liquid chromatography analysis (R2 = 0.99).

Keywords: (1)H NMR quantification; Dimethyl carbonate; Glycerol; Glycerol carbonate; Quantitative nuclear magnetic resonance.

MeSH terms

  • Carbonates / chemistry*
  • Esterification
  • Formates / chemistry
  • Glycerol / chemistry*
  • Proton Magnetic Resonance Spectroscopy
  • Solvents / chemistry

Substances

  • Carbonates
  • Formates
  • Solvents
  • methyl carbonate
  • Glycerol