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Design, Execution, and Analysis of Time-Varying Experiments for Model Discrimination and Parameter Estimation in Microreactors

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    Design, Execution, and Analysis of Time-Varying Experiments for Model Discrimination and Parameter Estimation in Microreactors
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    Department of Chemical Engineering, Massachusetts Institute of Technology, Cambridge, Massachusetts 02139, United States
    *E-mail: [email protected]
    *E-mail: [email protected]
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    Organic Process Research & Development

    Cite this: Org. Process Res. Dev. 2014, 18, 11, 1461–1467
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    https://doi.org/10.1021/op500179r
    Published September 8, 2014
    Copyright © 2014 American Chemical Society
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    Abstract

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    Time-varying, or dynamic, experiments can produce richer data sets than sequences of steady-state experiments using less material and time. A case study demonstrating this concept for microreactor experiments is presented. Beginning with five kinetic model candidates for the reaction of phenylisocyanate with t-butanol, an initial dynamic experiment showed that two of the five models gave a similar quality of fit to the experimental data, whereas the remaining three gave significantly poorer fits. Next an optimal experiment was designed to discriminate between the remaining two models. This drove the two models to differ significantly in quality, leaving a single model and a set of kinetic parameter values that adequately described the data. This method can be applied to future kinetic studies to reduce material use and experimental time while validating a dynamic model of the physics and chemical kinetics.

    Copyright © 2014 American Chemical Society

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    Supporting Information

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    Details of experimental and computational procedures; NMR spectra for PhNHBoc. This material is available free of charge via the Internet at http://pubs.acs.org.

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    Organic Process Research & Development

    Cite this: Org. Process Res. Dev. 2014, 18, 11, 1461–1467
    Click to copy citationCitation copied!
    https://doi.org/10.1021/op500179r
    Published September 8, 2014
    Copyright © 2014 American Chemical Society
    Request reuse permissions

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