skip to main content

Title: A reactor for high-throughput high-pressure nuclear magnetic resonance spectroscopy

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:
; ;  [1]
  1. Department of Chemistry, University of Wisconsin-Madison, Madison, Wisconsin 53719 (United States)
Publication Date:
OSTI Identifier:
22482569
Resource Type:
Journal Article
Resource Relation:
Journal Name: Review of Scientific Instruments; Journal Volume: 86; Journal Issue: 10; Other Information: (c) 2015 AIP Publishing LLC; Country of input: International Atomic Energy Agency (IAEA)
Country of Publication:
United States
Language:
English
Subject:
46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND TECHNOLOGY; DISSOLVED GASES; LIQUIDS; MONITORING; NUCLEAR MAGNETIC RESONANCE; PRESSURE RANGE MEGA PA 10-100; SAPPHIRE; WISCONSIN