Experimental aspects in acquisition of wide bandwidth solid-state MAS NMR spectra of low-γ nuclei with different opportunities on two commercial NMR spectrometers

[Display omitted] ► Wideband MAS NMR spectra of low-γ nuclei on Varian and Bruker NMR spectrometers. ► Experimental and simulated 14N MAS NMR spectra of glycine. ► Electronic measurements and simulations of circuitries for two different preamplifiers. ► Different opportunities for wideband MAS NMR s...

Ausführliche Beschreibung

Gespeichert in:
Bibliographische Detailangaben
Veröffentlicht in:Journal of magnetic resonance (1997) 2011-08, Vol.211 (2), p.195-206
Hauptverfasser: Jakobsen, Hans J., Bildsøe, Henrik, Gan, Zhehong, Brey, William W.
Format: Artikel
Sprache:eng
Schlagworte:
Online-Zugang:Volltext
Tags: Tag hinzufügen
Keine Tags, Fügen Sie den ersten Tag hinzu!
Beschreibung
Zusammenfassung:[Display omitted] ► Wideband MAS NMR spectra of low-γ nuclei on Varian and Bruker NMR spectrometers. ► Experimental and simulated 14N MAS NMR spectra of glycine. ► Electronic measurements and simulations of circuitries for two different preamplifiers. ► Different opportunities for wideband MAS NMR spectra of low-γ nuclei. The acquisition and different appearances observed for wide bandwidth solid-state MAS NMR spectra of low-γ nuclei, using 14N as an illustrative nucleus and employing two different commercial spectrometers (Varian, 14.1 T and Bruker, 19.6 T), have been compared/evaluated and optimized from an experimental NMR and an electronic engineering point of view, to account for the huge differences in these spectra. The large differences in their spectral appearances, employing the recommended/standard experimental set-up for the two different spectrometers, are shown to be associated with quite large differences in the electronic design of the two types of preamplifiers, which are connected to their respective probes through a 50 Ω cable, and are here completely accounted for. This has led to different opportunities for optimum performances in the acquisition of nearly ideal wide bandwidth spectra for low-γ nuclei on the two spectrometers by careful evaluation of the length for the 50 Ω probe-to-preamp cable for the Varian system and appropriate changes to the bandwidth ( Q) of the NMR probe used on the Bruker spectrometer. Earlier, we reported quite distorted spectra obtained with Varian Unity INOVA spectrometers (at 11.4 and 14.1 T) in several exploratory wide bandwidth 14N MAS NMR studies of inorganic nitrates and amino acids. These spectra have now been compared/evaluated with fully analyzed 14N MAS spectra correspondingly acquired at 19.6 T on a Bruker spectrometer. It is shown that our upgraded version of the STARS simulation/iterative-fitting software is capable of providing identical sets for the molecular spectral parameters and corresponding fits to the experimental spectra, which fully agree with the electronic measurements, despite the highly different appearances for the MAS NMR spectra acquired on the Varian and Bruker spectrometers.
ISSN:1090-7807
1096-0856
DOI:10.1016/j.jmr.2011.05.015