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

• DOI: 10.1007/s00723-014-0522-x
• Publication Date: 2014-02-25T10:52:06Z
• Authors: Franz Dalitz; Lennart Kreckel; Michael Maiwald; Gisela Guthausen
• Keywords: Spectral resolution; Robustness

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.