Dalligos Desiree M, Pilling Michael J, Dimitrakis Georgios, Ball Liam T
Department of Chemical and Environmental Engineering, University of Nottingham, Coates Building, Nottingham NG7 2RD, U.K.
School of Chemistry, University of Nottingham, Nottingham NG7 2RD, U.K.
Org Process Res Dev. 2023 May 30;27(6):1094-1103. doi: 10.1021/acs.oprd.3c00081. eCollection 2023 Jun 16.
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.
本文展示了宽带介电谱（DS）作为在线（原位）反应监测工具的适用性。以4-硝基苯酚的酯化反应作为测试案例，我们表明，使用同轴浸入式探头在宽频率范围内收集时间分辨的DS数据，并进行多变量分析，可以高精度、高准确度地测量反应进程。除了数据收集和分析工作流程外，我们还建立了一种便捷的方法，用于快速评估DS对以前未测试过的反应或过程的适用性。我们设想，鉴于其与其他光谱方法的正交性、低成本以及易于实施的特点，DS将成为过程化学家分析工具箱中的一项有价值的补充。
