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Gas bubbles in the NMR tube: an easy way to investigate reactions with gases in the liquid phase
Author(s) -
Baumann Wolfgang,
Mansel Stefan,
Heller Detlef,
Borns Susanne
Publication year - 1997
Publication title -
magnetic resonance in chemistry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.483
H-Index - 72
eISSN - 1097-458X
pISSN - 0749-1581
DOI - 10.1002/(sici)1097-458x(199711)35:10<701::aid-omr160>3.0.co;2-q
Subject(s) - chemistry , gas phase , ethylene , rhodium , liquid phase , carbon 13 nmr , diffusion , isobaric process , olefin fiber , nmr spectra database , proton nmr , phase (matter) , kinetics , analytical chemistry (journal) , catalysis , spectral line , organic chemistry , thermodynamics , physics , quantum mechanics , astronomy
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 ( 1 H, 13 C, 31 P) 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 olefin 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 influence of diffusion (stationary conditions). © 1997 John Wiley & Sons, Ltd.