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

Journal of magnetic resonance (San Diego, Calif. : 1997) (2011-06-28)
Hans J Jakobsen, Henrik Bildsøe, Zhehong Gan, William W Brey
ABSTRACT

The acquisition and different appearances observed for wide bandwidth solid-state MAS NMR spectra of low-γ nuclei, using (14)N as an illustrative nucleus and employing two different commercial spectrometers (Varian, 14.1T and Bruker, 19.6T), 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 50Ω 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 50Ω 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 14.1T) in several exploratory wide bandwidth (14)N MAS NMR studies of inorganic nitrates and amino acids. These spectra have now been compared/evaluated with fully analyzed (14)N MAS spectra correspondingly acquired at 19.6T 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.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Lead(II) nitrate, ACS reagent, ≥99.0%
Sigma-Aldrich
Lead(II) nitrate, 99.999% trace metals basis
Sigma-Aldrich
Lead(II) nitrate, ≥99.95% trace metals basis