Beach N J, Knapp S M M, Landis C R
Department of Chemistry, University of Wisconsin-Madison, Madison, Wisconsin 53719, USA.
Rev Sci Instrum. 2015 Oct;86(10):104101. doi: 10.1063/1.4932676.
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.
本文描述了一种用于高压气液反应的原位核磁共振（NMR）监测的反应器设计。威斯康星高压核磁共振反应器（WiHP-NMRR）设计包括四个模块：一个配有钛管支架的蓝宝石NMR管，该钛管支架额定压力高达1000 psig（68 atm），温度范围为-90至90°C；一个气体循环系统，可在消耗气体或释放气体的反应过程中维持溶解气体的平衡浓度；一个液体注入装置，能够在高压条件下向反应器中添加定量的溶液；以及一个快速清洗系统，可在不移出NMR仪器的情况下对反应器进行清洗。WiHP-NMRR与商用10 mm NMR探头兼容。在WiHP-NMRR中进行的反应在整个反应时间过程中可产生高质量、信息丰富的多核NMR数据，且实验周转迅速。
