Abstract
Non-invasive confocal Raman spectroscopy has been integrated into a highly controllable tri-segmented flow crystallisation environment to uncover the crystallisation pathway from nucleation to crystal growth of the polymorphic compound succinic acid.
Highlights
We present the optimisation of non-invasive Raman spectroscopy for the use in following the crystallisation profile of succinic acid
To optimise the implementation of non-invasive Raman spectroscopy into a tri-segmented flow crystallisation set-up, pre-prepared high density slurries of the polymorphs of PCM and succinic acid (SA) were initially investigated in a short reactor set-up
Scheme 1 shows the molecular structures of the materials of interest and the fluoroethylene propylene (FEP) tubing used as the reactor body
Summary
We present the optimisation of non-invasive Raman spectroscopy for the use in following the crystallisation profile of succinic acid. Raman spectroscopy, and in particular surface enhanced Raman spectroscopy (SERS), has been used to great effect in microfluidic environments as an analytical probe for solute concentration determination.[7] By employing segmented flow with nanoparticles either pre-prepared[8,9,10] or synthesised in flow,[11,12] the detection limit of the Raman can be greatly enhanced whilst the use of segmented flow simultaneously ensures there is no poisoning of the SERS substrate and provides plug flow.[13] This requires the introduction of nanoparticles that can greatly affect a crystallising system For this reason, analysis of crystallising solutions is not compatible with SERS
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