Gas bubbles in the NMR tube: an easy way to investigate reactions with gases in the liquid phase
✍ Scribed by Wolfgang Baumann; Stefan Mansel; Detlef Heller; Susanne Borns
- Publisher
- John Wiley and Sons
- Year
- 1997
- Tongue
- English
- Weight
- 328 KB
- Volume
- 35
- Category
- Article
- ISSN
- 0749-1581
No coin nor oath required. For personal study only.
✦ Synopsis
An easily accessible device for the study of reactions with gases in the liquid phase, consisting of a 10 mm NMR tube with a gas inlet, is presented. This arrangement serves for reaction monitoring and mechanistic studies by acquiring NMR spectra (1H, 13C, 31P) with a resolution that allows one to observe and characterize intermediates that cannot be isolated as pure substances. The quantity of the gas to be consumed is not limited. Examples from organometallic chemistry are presented : the formation of a zirconacyclopentene from a zirconium-alkyne complex and ethylene and investigations on rhodium-catalysed oleÐn hydrogenation. The qualitative and quantitative evaluation of the measurements and application to reaction kinetics are discussed. An uptake of 0.1 ml of gas per minute at normal pressure (isobaric) is possible without a marked inÑuence of di †usion (stationary conditions). 1997 ( John Wiley & Sons, Ltd.