On-Line Analysis of a Continuous-Flow Ozonolysis Reaction Using Raman Spectroscopy

Abstract

We describe the use of an on-line Raman analyzer to quantitatively track the levels of trans-stilbene, benzaldehyde, and alpha-methoxybenzyl hydroperoxide in a continuous flow ozonolysis reactor. Quantitative analysis is carried out using spectral stripping in order to overcome baseline artifacts inherent in simple peak area determinations and to incorporate prior knowledge into the analytical model. The performance of spectral stripping is compared to partial least squares (PLS) analysis. The effect of two process variables, feed flow rate and ozone concentration, are also explored. Finally, the benefit of utilizing an on-line technique is illustrated by demonstrating the bias introduced by sampling for off-line analysis.

Managing Hazardous Reactions and Compounds in Process Chemistry

“…The use of IR helps marry the rate of ozonolysis production with reaction rate and amount of the alkene present as it is introduced in a stream (306). Raman has also been used to monitor the reaction (307).…”

Raman Spectroscopy

“…Several pharmaceuticals are manufactured using an ozonolysis step, which can be readily tracked with Raman spectroscopy [184] . Pelletier et al demonstrated continuous quantitative concentration measurement of trans -stilbene reacting to give benzaldehyde and α -methoxybenzyl hydroperoxide, a model reaction [184] .…”

Adapting the chemical unfolding assay for high-throughput protein screening using experimental and spectroscopic corrections

“…A computational approach introduced in this work for the removal of light scattering is based on automated interference subtraction methods often used in the spectral domain [ 20 , 21 ]. These methods adjust the amount of an interfering profile until the first- or second-derivative of the spectral profile is at a minimum (i.e.…”