Issue 5, 2003

Mobile phase compensation to improve NMR spectral properties during solvent gradients

Abstract

A solvent compensation method based on flow injection analysis is used to obtain high quality nuclear magnetic resonance (NMR) spectra during solvent gradients. Using a binary solvent system containing D2O and CD3OD, NMR line broadening and chemical shift changes are observed with a 10% methanol per min solvent composition gradient. However, by creating a second equal but reverse gradient and combining the two solvent gradients before the NMR detector, the composition of solvent reaching the NMR flow cell is kept constant. We demonstrate a system using flow injection analysis of combining solvent gradients and show constant NMR spectral performance as a function of time as the combined flow has a constant solvent composition irrespective of the initial solvent gradient. Using this approach, methods can be developed to measure high quality NMR spectra during on-flow gradient LC-NMR experiments. The ultimate ability of this approach depends on the ability to compensate for the disturbance of the solvent gradient and reverse gradient by a pair of LC columns (the analytical and reverse gradient columns).

Article information

Article type
Paper
Submitted
04 Feb 2003
Accepted
02 Apr 2003
First published
22 Apr 2003

Analyst, 2003,128, 421-426

Mobile phase compensation to improve NMR spectral properties during solvent gradients

D. A. Jayawickrama, A. M. Wolters and J. V. Sweedler, Analyst, 2003, 128, 421 DOI: 10.1039/B301359F

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