Design, development, and analysis of an automated sampling loop for online monitoring of chiral crystallization
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Author (Corporation)
Publication date
15.02.2022
Type of student thesis
Course of study
Type
01A - Journal article
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Editor (Corporation)
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Parent work
Organic Process Research & Development
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Volume
26
Issue / Number
4
Pages / Duration
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Publisher / Publishing institution
American Chemical Society
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Abstract
Enantiomeric purity is of prime importance for several industries, specifically in the production of pharmaceuticals. Crystallization processes can be used to obtain pure enantiomers in a suitable solid form. However, some process variants inherently rely on kinetic enhancement (preferential crystallization) of the desired enantiomer or on complex interactions of several phenomena (e.g., attrition-enhanced deracemization and Viedma ripening). Thus, a process analytical technology able to measure the enantiomeric composition of both the solid phase and the liquid phase would be valuable to track and eventually control such processes. This study presents the design and development of a novel automated analytical monitoring system that achieves this. The designed setup tracks the enantiomeric excess (ee) using a continuous closed-loop sampling loop that is coupled to a polarimeter and an attenuated total reflection Fourier transform infrared spectroscopy spectrometer. By heating the loop and alternately sampling either the liquid or the suspension, the combination of these measurements allows tracking of the ee of both the liquid and the solid. This work demonstrates a proof of concept of both the experimental and theoretical aspects of the new system.
Keywords
Computer simulations, Crystallization, Liquids, Molecular structure, Suspensions
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ISBN
ISSN
1083-6160
1520-586X
1520-586X
Language
English
Created during FHNW affiliation
No
Strategic action fields FHNW
Publication status
Published
Review
Peer review of the complete publication
Open access category
Hybrid
License
Citation
Rehman, G. u., Vetter, T., & Martin, P. A. (2022). Design, development, and analysis of an automated sampling loop for online monitoring of chiral crystallization. Organic Process Research & Development, 26(4). https://doi.org/10.1021/acs.oprd.1c00320