Design, validation, and implementation of a rapid-injection NMR system.
A Rapid Injection NMR (RINMR) apparatus has been designed and constructed to allow the observation of fast chemical reactions in real time by NMR spectroscopy. The instrument was designed to allow the rapid (<2 s) injection and mixing of a metered volume of a reagent into a spinning NMR tube followed by rapid acquisition of the data resulting from the evolution of the chemical process. The various design criteria for this universal system included the ability to deliver any chemical reagent at any temperature and allow for the observation of any nucleus. The various challenges associated with the construction and implementation of this instrument are documented along with the validation of the accuracy of the apparatus with respect to volume and temperature. Finally, the ultimate validation and reproducibility of the technique is presented in the form of three case studies that used the instrument to elucidate various aspects of organic reaction mechanisms. The authors urge interested parties to not embark on the construction of their own instrument and invite those whose research problems might be amenable to this kind of analysis to contact the corresponding author for access to the apparatus described herein.
Denmark
Scott E
SE
Roger Adams Laboratory, Department of Chemistry, University of Illinois, Urbana, Illinois 61801, USA. sdenmark@illinois.edu
Williams
Bruce J
BJ
Eklov
Brian M
BM
Pham
Son M
SM
Beutner
Gregory L
GL
D002138:Calibration; D004867:Equipment Design; D004987:Ethers / Q000138:chemical synthesis / Q000737:chemistry; D009682:Magnetic Resonance Spectroscopy / Q000295:instrumentation* / Q000379:methods*; D015394:Molecular Structure; D012821:Silanes / Q000737:chemistry; D013237:Stereoisomerism; D013696:Temperature
D004987:Ethers; D012821:Silanes; C065893:trichlorosilane