Continuous flow H-1 and C-13 NMR spectroscopy in microfluidic stripline NMR chips
| Autor: | Roald M. Tiggelaar, P. Jan M. van Bentum, Anna Jo Oosthoek-de Vries, Arno P. M. Kentgens, Han Gardeniers, Jacob Bart, J.W.G. Janssen |
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| Přispěvatelé: | Mesoscale Chemical Systems |
| Rok vydání: | 2017 |
| Předmět: |
Chemistry
Continuous flow Microfluidics Detector Analytical chemistry 02 engineering and technology 010402 general chemistry 021001 nanoscience & nanotechnology Solid State NMR 01 natural sciences Article 0104 chemical sciences Analytical Chemistry Volumetric flow rate 13c nmr spectroscopy Heteronuclear molecule Magnet 0210 nano-technology GeneralLiterature_REFERENCE(e.g. dictionaries encyclopedias glossaries) Stripline |
| Zdroj: | Analytical Chemistry Analytical chemistry, 89(4), 2296-2303. American Chemical Society Analytical Chemistry, 89, 4, pp. 2296-2303 Analytical Chemistry, 89, 2296-2303 |
| ISSN: | 0003-2700 |
| Popis: | Microfluidic stripline NMR technology not only allows for NMR experiments to be performed on small sample volumes in the submicroliter range, but also experiments can easily be performed in continuous flow because of the stripline's favorable geometry. In this study we demonstrate the possibility of dual-channel operation of a microfluidic stripline NMR setup showing one- and two-dimensional 1H, 13C and heteronuclear NMR experiments under continuous flow. We performed experiments on ethyl crotonate and menthol, using three different types of NMR chips aiming for straightforward microfluidic connectivity. The detection volumes are approximately 150 and 250 nL, while flow rates ranging from 0.5 μL/min to 15 μL/min have been employed. We show that in continuous flow the pulse delay is determined by the replenishment time of the detector volume, if the sample trajectory in the magnet toward NMR detector is long enough to polarize the spin systems. This can considerably speed up quantitative measurement of samples needing signal averaging. So it can be beneficial to perform continuous flow measurements in this setup for analysis of, e.g., reactive, unstable, or mass-limited compounds. |
| Databáze: | OpenAIRE |
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