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Published on: July 9, 2021
Convection compensation in 3D iDOSY-HMBC 1H-13C-correlation experiments
Harri Heikkinen1, Ilkka Kilpeläinen2, Sami Heikkinen2
1Finnish Institute for Verification of the Chemical Weapons Convention (VERIFIN), Department of Chemistry, University of Helsinki, P.O. Box 55, FIN-00014 Helsinki, Finland.
Abstract:
3D iDOSY-HMBC (3D incorporated Diffusion Ordered SpectroscopY-Heteronuclear Multiple Bond Correlation) pulse sequences were modified to incorporate convection compensation element. No additional delays were required, and convection compensation was directly constructed within the existing delay periods in 3D iDOSY-HMBC pulse sequence. Convection compensation was achieved by pulsed field gradient double echo, thus avoiding the intensity loss normally related to stimulated echo methods. The incorporated convection compensation element improves the usability of 3D iDOSY-HMBC. In case of elevated temperatures, thermal convection leads to loss of resolution in DOSY-dimension or even to severe decrease of signal intensity, thus making convection uncompensated 3D iDOSY-HMBC infeasible. Aforementioned problems can be circumvented via utilization of the presented convection compensated 3D iDOSY-HMBC-versions.
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