Abstract

Developing A Compact, Portable 4.7 T Driven NMR System for At-Line Reaction Monitoring

David Strand, President & CEO, Protasis Corporation

We describe a first-of-kind, high-resolution NMR system based on a novel 4.7T (1H frequency 200MHz) high-temperature superconducting HTS-110 magnet, cooled by a standard helium compressor, driven by a high-stability power supply, and utilizing a new state-of-the-art RS2D single-board spectrometer. The system is designed to be portable, allowing for rapid cooling and ramping of the magnet to field without the need for expensive cryogens or a trained engineer. All system components except for the cryocooler pump are contained in a 72” x 28”D x 42”H portable cart with an expansive work surface. We have been using this system, installed at Pfizer Global R&D (Groton, CT), coupled with a Protasis microcoil flow probe to investigate a multitude of samples, ranging from traditional organic compounds to complex reaction mixtures. In particular, 1D 1H NMR spectra have been acquired during the time-course of ongoing reactions in small stirred-tank chemical reactors. We are also working toward utilizing more sophisticated multi-dimensional gradient-based experiments on this system to provide additional information on reaction mixtures in both a “stop-flow” and flow-through mode. This system works well for reaction monitoring, as it provides intermediate resolution between lower resolution 60 MHz spectrometers and traditional higher-field superconducting spectrometers at 400 MHz and above. This talk will provide an overview of this new technology and demonstrate the data we are able to achieve. The potential future role for NMR in chemical process control will be discussed.