Issue 11, 2021

A robust new tool for online solution-phase sampling of crystallizations

Abstract

Current PAT tools struggle to provide real time solid-phase composition data for crystallizations. HPLC offers a variety of benefits over other solution-phase PATs and can be used to infer solid-phase composition when combining total (solid plus solution phase) sampling with solution-only sampling. However, the selective solution-phase sampling of supersaturated solutions is extremely challenging. We herein present a dynamically flushed in situ filtration device that attaches to the tip of Mettler-Toledo's EasySampler probe and makes use of its mechanical motion to avoid surface fouling. Filter functionality was tested under both increasing saturation (via cooling or antisolvent addition) as well as decreasing saturation (via heating or solvent addition), illustrating its accuracy, reliability and versatility. The utility of the filter tip was highlighted by monitoring the classical resolution of TBZ, an important drug precursor.

Graphical abstract: A robust new tool for online solution-phase sampling of crystallizations

Supplementary files

Article information

Article type
Paper
Submitted
14 Jul 2021
Accepted
24 Aug 2021
First published
24 Aug 2021

React. Chem. Eng., 2021,6, 2042-2049

A robust new tool for online solution-phase sampling of crystallizations

A. J. Kukor, M. A. Guy, J. M. Hawkins and J. E. Hein, React. Chem. Eng., 2021, 6, 2042 DOI: 10.1039/D1RE00284H

To request permission to reproduce material from this article, please go to the Copyright Clearance Center request page.

If you are an author contributing to an RSC publication, you do not need to request permission provided correct acknowledgement is given.

If you are the author of this article, you do not need to request permission to reproduce figures and diagrams provided correct acknowledgement is given. If you want to reproduce the whole article in a third-party publication (excluding your thesis/dissertation for which permission is not required) please go to the Copyright Clearance Center request page.

Read more about how to correctly acknowledge RSC content.

Social activity

Spotlight

Advertisements