Development of low-field flow 31P NMR spectroscopy for reaction monitoring in organometallic chemistry Nuclear magnetic resonance Tadiello, Laura , 1996- (VerfasserIn) Beweries, Torsten , 1982- (AkademischeR BetreuerIn) Corzilius, Björn , 1979- (AkademischeR BetreuerIn) Universität Rostock (Grad-verleihende Institution) Universität Rostock Mathematisch-Naturwissenschaftliche Fakultät (Grad-verleihende Institution) Text theses Text Hochschulschrift 2024 2024 eng electronic resourceremoteComputermedienOnline-Ressourceapplication/pdf1 Online-Ressource (xvi, 121 Seiten) Illustrationen, Diagramme Benchtop low-field (LF) NMR spectroscopy is a valuable tool for reaction monitoring and its application in catalysis. It is particularly attractive thanks to its low-cost and portability (i.e., the instrument can be installed right next to the fume hood). However, crucial quantitative results, e.g., kinetic profiles, cannot be correctly determined the moment degradation of an air- and moisture-sensitive catalyst occurs. Therefore, inertness of the entire setup must be guaranteed. In the first part of this thesis, it is demonstrated that this challenge could be overcome to meet the experimental requirements of highly oxygen-sensitive rhodium diphosphine complexes, relevant for homogeneous catalysis. Indeed, a commercially available benchtop LF NMR spectrometer has been evolved into an inert customized flow setup. Catalytic hydrogenation monitoring via LF 1H and 31P NMR spectroscopy proved to be suitable with this flow setup despite the relatively low concentration of the investigated species (ca. 10 mM). In the second part of the thesis, limitations due to the low magnetic field of the benchtop spectrometer (1.9 T) and the relative insensitivity of 31P compared to 1H nucleus have been faced. 31P NMR signal-to-noise ratios (SNRs) have been improved using advanced pulse sequences. Sensitive Homogeneous And Resolved PEaks in Real time (SHARPER) enhances 31P NMR signals by collapsing the target resonance into an extremely narrow singlet and eliminating the effects of field inhomogeneity. After demonstrating the advantage of this tool in static conditions (up to 10-fold enhancement factor on SNR), the customized on-line setup has been used to monitor a faster reaction (in the order of minutes), that could not be followed with traditional 31P NMR sequences.<eng> Open Access Urheberrechtsschutz 1.0 vorgelegt von Laura Tadiello GutachterInnen: Torsten Beweries (Leibniz-Institut für Katalyse e. V.) ; Björn Corzilius (Universität Rostock, Institut für Chemie) Dissertation Universität Rostock 2024 540 543 540 https://purl.uni-rostock.de/rosdok/id00004876 https://doi.org/10.18453/rosdok_id00004876 https://nbn-resolving.org/urn:nbn:de:gbv:28-rosdok_id00004876-1 https://d-nb.info/1373150661/34 Development of low-field flow 31P NMR spectroscopy for reaction monitoring in organometallic chemistry--(DE-627)1931404364 urn:nbn:de:gbv:28-rosdok_id00004876-1 doi: 10.18453/rosdok_id00004876 oclc: 1528456914 ppn: (DE-627)1931401799