Abstract
This chapter evaluates the application of quantitative high-resolution online nuclear magnetic resonance (NMR) spectroscopy for investigating complex reacting mixtures. It is the method of choice for the investigation of complex fluid mixtures with analytically similar compounds, where other analytical methods suffer from insufficient differentiation of components. Online coupling of NMR spectrometers was first developed with high-performance liquid chromatography (HPLC) and supercritical fluid chromatography (SFC), using NMR as an analytical detector with high spectral dispersion. Flow NMR probes were developed, and these have also been used for high-throughput NMR spectroscopy. A major advantage of NMR spectroscopy is that no calibration is needed for quantification in most cases, and the method features a high linearity between absolute signal area and sample concentration. Furthermore, online NMR spectroscopy allows investigations under elevated pressures, preventing the solutions from boiling, or for studies under process conditions. The use of flow NMR to monitor the concentration of chemical compartments during the course of a reaction is feasible and provides high-quality quantitative data. The reaction is allowed to progress under conditions that closely resemble the plant, and complex conditions can be accommodated. Future applications may also include deployment of such devices that use NMR detection in the chemical plant, sampling from the reaction itself in real time.
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