Traditional Nuclear Magnetic Resonance (NMR) instruments, although an extremely powerful characterization tool, is not conducive to incorporation as a process analytical technology (PAT). The realities of their footprint and the required frequent routine maintenance, paired with their expensive capital and operating expenditures have left this non-destructive, inherently quantitative technique out of online industrial processes. The recent developments of a new class of instrumentation, the benchtop NMR spectrometer, offers an interesting alternative with which to develop reliable continuous-flow analytical methods and incorporate this technique into improving chemical processes. Herein we discuss the design of a flow cell to acquire both stopped flow and continuous flow 1H, 19F and 31P NMR data. First we will show how laboratory reactions can be self-optimized using integrated feedback loops built into an accessible application programmatic interface (API). Next we will apply lessons learned in a controlled laboratory environment and highlight developments towards a hardened, ruggedized tool including considerations such as thermal control and explosion-proof casing.

Developments in monitoring continuous reactions by online benchtop NMR: Development of benchtop NMR as a process analytical technology

254th National Meeting (2017)

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