Abstract
FlowNMR spectroscopy is an excellent technique for non-invasive real-time reaction monitoring under relevant conditions that avoids many of the limitations that bedevil other reaction monitoring techniques.
Highlights
Reaction monitoring techniques may be coupled directly to a reaction vessel, with a probe inserted into the vessel or with the reaction vessel connected to the instrument via hyphenated tubing
A recent study by Foley et al clearly demonstrates the significance of mass transfer limitations when using static nuclear magnetic resonance (NMR) tubes for reaction monitoring, leading to strikingly different kinetic results for the same reaction when monitored by different NMR techniques.[2]
For all on-line NMR reaction monitoring setups there is an inherent time required for the sample to be pumped from the reaction vessel to the spectrometer, leading to a slight delay between a change occurring in the reaction vessel and detection
Summary
Practical aspects of real-time reaction monitoring using multi-nuclear high resolution FlowNMR spectroscopy†. FlowNMR spectroscopy is an excellent technique for non-invasive real-time reaction monitoring under relevant conditions that avoids many of the limitations that bedevil other reaction monitoring techniques. With the recent commercial availability of FlowNMR hard- and software solutions for high resolution spectrometers it is enjoying increased popularity in both academia and industry. We present an account on practical aspects of high field multi-nuclear FlowNMR for reaction monitoring including apparatus design, flow effects, acquisition parameters and data treatment, which are important to consider if accurate kinetic data are to be obtained from FlowNMR experiments. Flow effects on NMR peak areas are important as they can lead to large quantification errors if overlooked, but can be corrected for and even used to increase temporal resolution with suitably adjusted instrument settings
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