• Treffer 6 von 11
Zurück zur Trefferliste

Automated data evaluation and modelling of simultaneous F-19-H-1 medium-resolution NMR spectra for online reaction monitoring

  • Medium-resolution nuclear magnetic resonance spectroscopy (MR-NMR) currently develops to an important analytical tool for both quality control and processmonitoring. In contrast to high-resolution onlineNMR (HR-NMR),MR-NMRcan be operated under rough environmental conditions. A continuous re-circulating stream of reaction mixture fromthe reaction vessel to the NMR spectrometer enables a non-invasive, volume integrating online analysis of reactants and products. Here, we investigate the esterification of 2,2,2-trifluoroethanol with acetic acid to 2,2,2-trifluoroethyl acetate both by 1H HR-NMR (500MHz) and 1H and 19F MRNMR (43MHz) as amodel system. The parallel online measurement is realised by splitting the flow,which allows the adjustment of quantitative and independent flow rates, both in the HR-NMR probe as well as in the MR-NMR probe, in addition to a fast bypass line back to the reactor. One of the fundamental acceptance criteria for online MR-MNR spectroscopy is a robust dataMedium-resolution nuclear magnetic resonance spectroscopy (MR-NMR) currently develops to an important analytical tool for both quality control and processmonitoring. In contrast to high-resolution onlineNMR (HR-NMR),MR-NMRcan be operated under rough environmental conditions. A continuous re-circulating stream of reaction mixture fromthe reaction vessel to the NMR spectrometer enables a non-invasive, volume integrating online analysis of reactants and products. Here, we investigate the esterification of 2,2,2-trifluoroethanol with acetic acid to 2,2,2-trifluoroethyl acetate both by 1H HR-NMR (500MHz) and 1H and 19F MRNMR (43MHz) as amodel system. The parallel online measurement is realised by splitting the flow,which allows the adjustment of quantitative and independent flow rates, both in the HR-NMR probe as well as in the MR-NMR probe, in addition to a fast bypass line back to the reactor. One of the fundamental acceptance criteria for online MR-MNR spectroscopy is a robust data treatment and evaluation strategy with the potential for automation. The MR-NMR spectra are treated by an automated baseline and phase correction using the minimum entropy method. The evaluation strategies comprise (i) direct integration, (ii) automated line fitting, (iii) indirect hard modelling (IHM) and (iv) partial least squares regression (PLS-R). To assess the potential of these evaluation strategies for MR-NMR, prediction results are compared with the line fitting data derived from the quantitative HR-NMR spectroscopy. Although, superior results are obtained from both IHM and PLS-R for 1H MR-NMR, especially the latter demands for elaborate data pretreatment, whereas IHM models needed no previous alignment.zeige mehrzeige weniger

Volltext Dateien herunterladen

  • Zientek_Automated data evaluation.pdf
    eng

Metadaten exportieren

Weitere Dienste

Teilen auf Twitter Suche bei Google Scholar
Metadaten
Autoren/innen:Nicolai Zientek, C. Laurain, Klas MeyerORCiD, Andrea PaulORCiD, D. Engel, G. Guthausen, M. Kraume, Michael MaiwaldORCiD
Dokumenttyp:Zeitschriftenartikel
Veröffentlichungsform:Verlagsliteratur
Sprache:Englisch
Titel des übergeordneten Werkes (Englisch):Magnetic Resonance in Chemistry
Jahr der Erstveröffentlichung:2016
Organisationseinheit der BAM:1 Analytische Chemie; Referenzmaterialien
1 Analytische Chemie; Referenzmaterialien / 1.4 Prozessanalytik
Verlag:John Wiley & Sons, Ltd
Verlagsort:Hoboken, New Jersey, USA
Jahrgang/Band:54
Erste Seite:513
Letzte Seite:520
DDC-Klassifikation:Naturwissenschaften und Mathematik / Chemie / Analytische Chemie
Freie Schlagwörter:19F-NMR; 1H-NMR; Automation; Chemometrics; Data processing; IHM; Indirect hard modeling; Medium-resolution NMR; NMR; Online NMR; PLS-R; Partial least squares regression; Process analytical technology; Quantitative NMR; Reaction monitoring
Themenfelder/Aktivitätsfelder der BAM:Analytical Sciences
Analytical Sciences / Sensorik
DOI:https://doi.org/doi:10.1002/mrc.4216
URL:http://onlinelibrary.wiley.com/doi/10.1002/mrc.4216/abstract
URL:http://gateway.webofknowledge.com/gateway/Gateway.cgi?GWVersion=2&SrcAuth=Alerting&SrcApp=Alerting&DestApp=WOS&DestLinkType=FullRecord;UT=WOS:000379965900014
Verfügbarkeit des Dokuments:Datei im Netzwerk der BAM verfügbar ("Closed Access")
Datum der Freischaltung:23.05.2016
Referierte Publikation:Ja
Datum der Eintragung als referierte Publikation:15.08.2016