title: A reactor for high-throughput high-pressure nuclear magnetic resonance spectroscopy.
abstract: The design of a reactor for operando nuclear magnetic resonance (NMR) monitoring of high-pressure gas-liquid reactions is described. The Wisconsin High Pressure NMR Reactor (WiHP-NMRR) design comprises four modules: a sapphire NMR tube with titanium tube holder rated for pressures as high as 1000 psig (68 atm) and temperatures ranging from -90 to 90 °C, a gas circulation system that maintains equilibrium concentrations of dissolved gases during gas-consuming or gas-releasing reactions, a liquid injection apparatus that is capable of adding measured amounts of solutions to the reactor under high pressure conditions, and a rapid wash system that enables the reactor to be cleaned without removal from the NMR instrument. The WiHP-NMRR is compatible with commercial 10 mm NMR probes. Reactions performed in the WiHP-NMRR yield high quality, information-rich, and multinuclear NMR data over the entire reaction time course with rapid experimental turnaround.
authors.affiliation: Department of Chemistry, University of Wisconsin-Madison, Madison, Wisconsin 53719, USA.
authors.forename: N J
authors.initials: NJ
authors.lastname: Beach
authors.affiliation: Department of Chemistry, University of Wisconsin-Madison, Madison, Wisconsin 53719, USA.
authors.forename: S M M
authors.initials: SM
authors.lastname: Knapp
authors.affiliation: Department of Chemistry, University of Wisconsin-Madison, Madison, Wisconsin 53719, USA.
authors.forename: C R
authors.initials: CR
authors.lastname: Landis