Potential of vis-NIR spectroscopy to monitor the silica precipitation reaction

Anal Bioanal Chem. 2017 Jan;409(3):785-796. doi: 10.1007/s00216-016-0064-1. Epub 2016 Nov 28.

Abstract

Controlling production online is an important issue for chemical companies. Visible and near-infrared (NIR) spectroscopy offers a number of important advantages for process monitoring, and has been used since the 1980s. For complex media such as silica precipitation samples, it is interesting to be able to study independently the scattering and absorption effects. From the scattering coefficient it is possible to extract information on the physical structure of the medium. In this work, the physical changes were monitored during a silica precipitation reaction by simple measurement of collimated transmittance NIR spectra. It is shown that it is possible to differentiate samples before and after the gel point, which is a key parameter for monitoring the process. From these NIR spectra the scattering coefficients were simply extracted, allowing a global vision of the physical changes in the medium. Then principal component analysis of the spectra allowed refinement of the understanding of the scattering effects, in combination with particle size monitoring.

Keywords: Collimated transmission; Monitoring silica precipitation; Near-infrared spectroscopy; Physical properties; Scattering coefficients.