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Trading sensitivity for information: Carr–Purcell–Meiboom–Gill acquisition in solid-state NMR.

Authors :
Dey, Krishna K.
Ash, Jason T.
Trease, Nicole M.
Grandinetti, Philip J.
Source :
Journal of Chemical Physics; 8/7/2010, Vol. 133 Issue 5, p054501, 10p, 2 Diagrams, 4 Charts, 8 Graphs
Publication Year :
2010

Abstract

The Carr–Purcell–Meiboom–Gill (CPMG) experiment has gained popularity in solid-state NMR as a method for enhancing sensitivity for anisotropically broadened spectra of both spin 1/2 and half integer quadrupolar nuclei. Most commonly, the train of CPMG echoes is Fourier transformed directly, which causes the NMR powder pattern to break up into a series of sidebands, sometimes called “spikelets.” Larger sensitivity enhancements are observed as the delay between the π pulses is shortened. As the duration between the π pulses is shortened, however, the echoes become truncated and information about the nuclear spin interactions is lost. We explored the relationship between enhanced sensitivity and loss of information as a function of the product Ω 2τ, where Ω is the span of the anisotropic lineshape and 2τ is the π pulse spacing. For a lineshape dominated by the nuclear shielding anisotropy, we found that the minimum uncertainty in the tensor values is obtained using Ω 2τ values in the range Ω 2τ≈12<subscript>-1</subscript><superscript>+6</superscript> and Ω 2τ≈9<subscript>-3</subscript><superscript>+3</superscript> for η<subscript>s</subscript>=0 and η<subscript>s</subscript>=1, respectively. For an anisotropic second-order quadrupolar central transition lineshape under magic-angle spinning (MAS), the optimum range of Ω 2τ≈9<subscript>-2</subscript><superscript>+3</superscript> was found. Additionally, we show how the Two-dimensional One Pulse (TOP) like processing approach can be used to eliminate the cumbersome sideband pattern lineshape and recover a more familiar lineshape that is easily analyzed with conventional lineshape simulation algorithms. [ABSTRACT FROM AUTHOR]

Details

Language :
English
ISSN :
00219606
Volume :
133
Issue :
5
Database :
Complementary Index
Journal :
Journal of Chemical Physics
Publication Type :
Academic Journal
Accession number :
52802711
Full Text :
https://doi.org/10.1063/1.3463653