English

Improved sensitivity and quantification for ${}^{29}$Si NMR experiments on solids using UDEFT (Uniform Driven Equilibrium Fourier Transform)

Materials Science 2020-03-10 v1 Chemical Physics

Abstract

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 29{}^{29}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 29{}^{29}Si-enriched amorphous silica and borosilicate glass, we show that 59180{}_{180}2980{}_{0}59180{}_{180} refocusing composite π\pi-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 cycling limit the pulse imperfections and the artifacts produced by stimulated echoes. The sensitivity of SP, UDEFT and CPMG (Carr-Purcell Meiboom-Gill) techniques are compared experimentally on functionalized and non-functionalized mesoporous silica. Furthermore, experiments on a flame retardant material prove that UDEFT technique provides a better quantification of 29{}^{29}Si sites with higher sensitivity than SP method.

Cite

@article{arxiv.2003.03624,
  title  = {Improved sensitivity and quantification for ${}^{29}$Si NMR experiments on solids using UDEFT (Uniform Driven Equilibrium Fourier Transform)},
  author = {Nghia Tuan Duong and Julien Trébosc and Olivier Lafon and Jean-Paul Amoureux},
  journal= {arXiv preprint arXiv:2003.03624},
  year   = {2020}
}
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