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Quantitative Medium-Resolution NMR Spectroscopy Under Non-Equilibrium Conditions, Studied on the Example of an Esterification Reaction

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Abstract

Medium-resolution nuclear magnetic resonance spectroscopy is a promising tool for the monitoring of liquid reactions. For process analytical applications, the requirements of robustness and insensitivity of the spectrometer in relation to high temperatures and pressures are challenging. Within this study, a flow probe using a glass dewar is presented. Temperatures of flowing samples up to 130 °C and pressures up to 40 bar were successfully applied, and the corresponding temperature loss of the flowing sample at 2 ml min−1 was <2.4 °C at 130 °C. Furthermore, if the process requires a measurement in a non-equilibrium state of magnetization, a comprehensive data treatment is given. For this purpose, the influences of the flow and T 1 of the substances under investigation are studied in detail on the example of a homogeneously catalyzed esterification. In addition, data analysis schemes were designed such that the experiments directly revealed mole fractions from the spectra. Limited spectral resolutions and low signal-to-noise ratio still did not obstruct quantitative interpretation of the experiments.

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Acknowledgments

The DFG is gratefully acknowledged for providing financial support for the instrumental facility center Pro2NMR as well as for the project on medium resolution NMR spectroscopy at KIT and BAM. Additionally, the assistance of P. Teppert and B. Schuhmann during the experiments is gratefully acknowledged.

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Authors and Affiliations

  1. Pro²NMR, Institute of MVM and IBG2, Karlsruhe Institute of Technology (KIT), Adenauerring 20b, 76131, Karlsruhe, Germany

    Franz Dalitz, Lennart Kreckel & Gisela Guthausen

  2. BAM Federal Institute for Materials Research and Testing, Richard-Willstaetter-Str. 11, 12489, Berlin, Germany

    Michael Maiwald

Authors
  1. Franz Dalitz
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  2. Lennart Kreckel
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  3. Michael Maiwald
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  4. Gisela Guthausen
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Correspondence to Gisela Guthausen.

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Dalitz, F., Kreckel, L., Maiwald, M. et al. Quantitative Medium-Resolution NMR Spectroscopy Under Non-Equilibrium Conditions, Studied on the Example of an Esterification Reaction. Appl Magn Reson 45, 411–425 (2014). https://doi.org/10.1007/s00723-014-0522-x

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  • DOI: https://doi.org/10.1007/s00723-014-0522-x

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