Raman Spectral Analysis for Quality Determination of Grignard Reagent

Abstract

Grignard reagent is one of the most popular materials in chemical and pharmaceutical reaction processes, and requires high quality with minimal adulteration. In this study, Raman spectroscopic technique was investigated for the rapid determination of toluene content, which is one of the common adulterants in Grignard reagent. Raman spectroscopy is the most suitable spectroscopic method to mitigate moisture and CO2 interference in the molecules of Grignard reagent. Raman spectra for the mixtures of toluene and Grignard reagent with different concentrations were analyzed with a partial least square regression (PLSR) method. The combination of spectral wavebands in the prediction model was optimized with a variables selection method of variable importance in projection (VIP). The results obtained from the VIP-based PLSR model showed the reliable performance of Raman spectroscopy for predicting the toluene concentration present in Grignard reagent with a correlation coefficient value of 0.97 and a standard error of prediction (SEP) of 0.71%. The results showed that Raman spectroscopy combined with multivariate analysis could be an effective analytical tool for rapid determination of the quality of Grignard reagent.

Keywords

• Grignard reagent
• chemical adulteration
• Raman spectroscopy
• variable importance in projection
• multivariate analysis
• quality determination