Identification and quantification of diethylene glycol contamination in glycerine raw material

Abstract

Fourier-transform infrared spectroscopy (FTIR) was successfully used for quantitative determination of diethylene glycol in glycerin raw material. In addition to the pure samples of both diethylene glycol and glycerin, nine binary mixtures of the two components with mixing ratios ranging from (70 to 98)%wt were created and studied as a training set. Glycerine showed, thereby, characteristic infrared bands at 1110, 992, 974, and 922 cm⁻¹ while those of diethylene glycol appear at 1085, 887, and 881 cm⁻¹. The quantitative determination of diethylene glycol in binary mixtures with glycerin was achieved upon using the absorbance difference between the 992 cm⁻¹ and the 881 cm⁻¹ as well as between 1110 and 1085 cm⁻¹ bands. With an average %error of 0.60 and 1.74, respectively and a limit of detection down to 0.85%, the created calibration curves from the training set were applied successfully to determine the composition of another eight binary mixtures of the two materials representing a validation set. The method was also applied to aqueous solutions of diethylene glycol and glycerin that contains (25 and 50)%wt water. Once more, training and validation sets of mixtures with different diethylene glycol and glycerin ratios at the two water percentages were prepared and measured. Again, successful determination of diethylene glycol in these aqueous solutions was achieved with an average %error of 0.92 and 0.47, respectively.

Keywords:

• FT-IR
• glycerine
• diethylene glycol