Quantitative NMR spectroscopy of technical mixtures and gases from elevated to high-pressure
- Recent technical developments of NMR instruments such as in acquisition electronics and probe design allow detection limits of components in liquid mixtures in the lower ppm range (approx.. 5–10 ppm amount of substance). The major advantage of quantitative NMR spectroscopy (qNMR) is that it is a direct ratio method of analysis without the need of calibration. This means that the signal for a specific NMR-active nucleus (e.g., a proton) in an analyte can be compared and quantified by reference to a different nucleus of a separate compound, comparable to a counting of spins in the active volume of the spectrometer.
Technical mixtures can be investigated online directly next to a process setup by using flow probes. This makes it a promising method for process analytical applications, especially during process development in laboratory and pilot plant scale. With the growing market of Benchtop devices based on permanent magnets nowadays an integration of NMR spectroscopy in an industrialRecent technical developments of NMR instruments such as in acquisition electronics and probe design allow detection limits of components in liquid mixtures in the lower ppm range (approx.. 5–10 ppm amount of substance). The major advantage of quantitative NMR spectroscopy (qNMR) is that it is a direct ratio method of analysis without the need of calibration. This means that the signal for a specific NMR-active nucleus (e.g., a proton) in an analyte can be compared and quantified by reference to a different nucleus of a separate compound, comparable to a counting of spins in the active volume of the spectrometer.
Technical mixtures can be investigated online directly next to a process setup by using flow probes. This makes it a promising method for process analytical applications, especially during process development in laboratory and pilot plant scale. With the growing market of Benchtop devices based on permanent magnets nowadays an integration of NMR spectroscopy in an industrial environment becomes reasonable.
A special application of qNMR in technical mixtures is the observation in the gas phase, which is rarely applied compared to liquid and solid NMR studies. Because of the low density it results in a reduced sensitivity, which can be improved by applying pressure. Therefore a high-pressure NMR setup was developed based on a commercially available NMR tube made of zirconia. This is currently tested up to 20 MPa, but can be extended up to 100 MPa with regard to pressure rating of its components. This work shows results of gas-phase application on natural-gas like reference gas mixtures produced at BAM, as well as investigations on liquefied gas mixtures with high accuracy provided in piston cylinders.
Besides that amine gas treatment and hydroformylation in a microemulsion represent two other examples of applications in process analytical technology. These show the potential of combination of online NMR spectroscopy with other spectroscopic methods, especially during model development for data evaluation.…
Autor*innen: | Klas MeyerORCiD |
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Weitere Person: | J.-P. Ruiken, B. Kraemer, M. Illner, D. Müller, E. Esche, Andrea PaulORCiD, G. Wozny, Michael MaiwaldORCiD |
Dokumenttyp: | Vortrag |
Veröffentlichungsform: | Präsentation |
Sprache: | Englisch |
Jahr der Erstveröffentlichung: | 2016 |
DDC-Klassifikation: | Naturwissenschaften und Mathematik / Chemie / Analytische Chemie |
Freie Schlagwörter: | Gas-phase NMR; Process analytical technology; Quantitative NMR spectroscopy |
Veranstaltung: | Presentation at Statoil Research Center |
Veranstaltungsort: | Trondheim, Norway |
Beginndatum der Veranstaltung: | 27.05.2016 |
Enddatum der Veranstaltung: | 27.05.2016 |
Verfügbarkeit des Dokuments: | Datei im Netzwerk der BAM verfügbar ("Closed Access") |
Datum der Freischaltung: | 02.06.2016 |
Referierte Publikation: | Nein |
Eingeladener Vortrag: | Nein |