4.6 Article

Coaxial Dielectric Spectroscopy as an In-Line Process Analytical Technique for Reaction Monitoring

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ORGANIC PROCESS RESEARCH & DEVELOPMENT
卷 27, 期 6, 页码 1094-1103

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AMER CHEMICAL SOC
DOI: 10.1021/acs.oprd.3c00081

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dielectric spectroscopy; reaction monitoring; process analytical technology; multivariate analysis

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The suitability of broadband dielectric spectroscopy (DS) for in-line reaction monitoring is demonstrated, showing high precision and accuracy in measuring reaction progress. A convenient method for rapidly assessing the applicability of DS to previously untested reactions or processes is also established. DS is seen as a valuable addition to the process chemist's analytical toolbox due to its orthogonality to other spectroscopic methods, low cost, and ease of implementation.
The suitability of broadband dielectric spectroscopy (DS) as a tool for in-line (in situ) reaction monitoring is demonstrated. Using the esterification of 4-nitrophenol as a test-case, we show that multivariate analysis of time-resolved DS data-collected across a wide frequency range with a coaxial dip-probe-allows reaction progress to be measured with both high precision and high accuracy. In addition to the workflows for data collection and analysis, we also establish a convenient method for rapidly assessing the applicability of DS to previously untested reactions or processes. We envisage that, given its orthogonality to other spectroscopic methods, its low cost, and its ease of implementation, DS will be a valuable addition to the process chemist's analytical toolbox.

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