Polarization transfer methods for quantitative analysis of flowing mixtures with benchtop 13C NMR spectroscopy

© 2023 The Authors. Magnetic Resonance in Chemistry published by John Wiley & Sons Ltd.

Bibliographische Detailangaben
Veröffentlicht in:Magnetic resonance in chemistry : MRC. - 1985. - 62(2024), 5 vom: 08. Apr., Seite 398-411
1. Verfasser: Phuong, Johnnie (VerfasserIn)
Weitere Verfasser: Romero, Zeno, Hasse, Hans, Münnemann, Kerstin
Format: Online-Aufsatz
Sprache:English
Veröffentlicht: 2024
Zugriff auf das übergeordnete Werk:Magnetic resonance in chemistry : MRC
Schlagworte:Journal Article 1H; 13C benchtop NMR flow NMR polarization transfer process monitoring quantitative analysis
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520 |a Benchtop NMR spectroscopy is attractive for process monitoring; however, there are still drawbacks that often hamper its use, namely, the comparatively low spectral resolution in 1H NMR, as well as the low signal intensities and problems with the premagnetization of flowing samples in 13C NMR. We show here that all these problems can be overcome by using 1H-13C polarization transfer methods. Two ternary test mixtures (one with overlapping peaks in the 1H NMR spectrum and one with well-separated peaks, which was used as a reference) were studied with a 1 T benchtop NMR spectrometer using the polarization transfer sequence PENDANT (polarization enhancement that is nurtured during attached nucleus testing). The mixtures were analyzed quantitatively in stationary as well as in flow experiments by PENDANT enhanced 13C NMR experiments, and the results were compared with those from the gravimetric sample preparation and from standard 1H and 13C NMR spectroscopy. Furthermore, as a proxy for a process monitoring application, continuous dilution experiments were carried out, and the composition of the mixture was monitored in a flow setup by 13C NMR benchtop spectroscopy with PENDANT. The results demonstrate the high potential of polarization transfer methods for applications in quantitative process analysis with benchtop NMR instruments, in particular with flowing samples 
650 4 |a Journal Article 
650 4 |a 1H; 13C 
650 4 |a benchtop NMR 
650 4 |a flow NMR 
650 4 |a polarization transfer 
650 4 |a process monitoring 
650 4 |a quantitative analysis 
700 1 |a Romero, Zeno  |e verfasserin  |4 aut 
700 1 |a Hasse, Hans  |e verfasserin  |4 aut 
700 1 |a Münnemann, Kerstin  |e verfasserin  |4 aut 
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