DETERMINATION OF RESIDUAL METHANOL AND ETHANOL IN BIODIESEL BY 1H-NMR

Abstract

Alcohol residues in biodiesel can be present even after the purification steps. It diminishes the flash point, lubricity and cetane number. The standard technique to quantify residual alcohol in biodiesel is the FID-GC with headspace sampling. NMR, although underused for quantitative analyses, requires no special sample preparation, and consumes low volume of solvent. In this work, methodologies for the residual methanol and ethanol contents in soy biodiesel by 1H-NMR in a 9.4 T (400 MHz) spectrometer by standard addition were developed and validated. Quantification limits were found equal to 0.07 and 0.08% respectively, so more than twice lower than the maximum level acceptable, which is 0.2%. Accuracy and precision were considered suitable for the alcohol content around the specification limit.