Ambient temperature 1H/13C NMR spectra of sodium 3-(trimethylsilyl)propane-1-sulfonate (DSS) in D2O referenced to external TMS A discussion of these and closely related results. Corrections for the bulk magnetic susceptibility effect for aqueous NMR samples

Ambient temperature 1H/13C NMR spectra of sodium 3-(trimethylsilyl)propane-1-sulfonate (DSS) in D2O referenced to external TMS : A discussion of these and closely related results. Corrections for the bulk magnetic susceptibility effect for aqueous NMR samples

© 2024 John Wiley & Sons Ltd.

Bibliographische Detailangaben
Veröffentlicht in:Magnetic resonance in chemistry : MRC. - 1985. - 62(2024), 7 vom: 27. Mai, Seite 535-543
1. Verfasser: Nazarski, Ryszard B (VerfasserIn)
Format: Online-Aufsatz
Sprache:English
Veröffentlicht: 2024
Zugriff auf das übergeordnete Werk:Magnetic resonance in chemistry : MRC
Schlagworte:Journal Article BMS shift GIAO method HOD signal NMR thermometer aqueous solutions external referencing magnetic susceptibility shape factor temperature calibration tetramethylsilane
Beschreibung
Zusammenfassung:© 2024 John Wiley & Sons Ltd.
This study aimed to obtain the title spectra and verify the temperature dependence of δDSS of the HOD signal from D2O of the NMR sample. However, the analysis of the collected δX data, extended by the results of other closely related measurements reported in the literature, provided important guidelines for performing routine 1H/13C NMR spectra in aqueous solvents externally referenced to neat liquid TMS contained in a coaxial capillary. Therefore, it is recommended that the previously proposed correction of δX data thus determined, which is mainly due to the difference in volume magnetic susceptibility χv between the sample and the external standard used, usually called the bulk magnetic susceptibility (BMS) correction, has been increased by +0.05 ppm (7%). The new value of this correction, +0.73 ppm, based on NMR experiments carried out at a standard temperature of 25°C, was confirmed in a classical approach using critically reviewed χm, χM, and ρ data for TMS, D2O, and H2O. The BMS correction for H2O solutions is +0.75 ppm. Important issues concerning magnetic susceptibility measurements for D2O and H2O, coaxial bulb-ended inserts, and the geometry of two-tube NMR cells (shape factor αav) are also critically discussed here, partly from a historical perspective
Beschreibung:Date Revised 29.05.2024
published: Print-Electronic
Citation Status PubMed-not-MEDLINE
ISSN:1097-458X
DOI:10.1002/mrc.5440