Improved sensitivity and quantification for Si NMR experiments on solids using UDEFT (Uniform Driven Equilibrium Fourier Transform).

Solid State Nucl Magn Reson

Univ. Lille, Centrale Lille, ENSCL, Univ. Artois, CNRS-8181, UCCS - Unit of Catalysis and Chemistry of Solids, F-59000 Lille, France; Bruker Biospin, 34 rue de l'industrie, F-67166 Wissembourg, France. Electronic address:

Published: August 2019

We demonstrate the possibility to use UDEFT (Uniform Driven Equilibrium Fourier Transform) technique in order to improve the sensitivity and the quantification of one-dimensional Si NMR experiments under magic-angle spinning (MAS). We derive an analytical expression of the signal-to-noise ratios of UDEFT and single-pulse (SP) experiments subsuming the contributions of transient and steady-state regimes. Using numerical spin dynamics simulations and experiments on Si-enriched amorphous silica and borosilicate glass, we show that 5929859 refocusing composite π-pulse and the adiabatic inversion using tanh/tan modulation improve the robustness of UDEFT technique to rf-inhomogeneity, offset, and chemical shift anisotropy. These pulses combined with a two-step phase cycle limit the pulse imperfections and the artifacts produced by stimulated echoes. The sensitivity of SP, UDEFT and CPMG (Carr-Purcell-Meiboom-Gill) techniques are experimentally compared on functionalized and non-functionalized mesoporous silica. Furthermore, experiments on a flame retardant material prove that UDEFT technique provides a better quantification of Si sites with higher sensitivity than SP method.

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http://dx.doi.org/10.1016/j.ssnmr.2019.03.007DOI Listing

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