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Low-load rotor-synchronised Hahn-echo pulse train (RS-HEPT) 1H decoupling in solid-state NMR: factors affecting MAS spin-echo dephasing times
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Griffin, John M., Tripon, Carmen, Samoson, Ago, Filip, Claudiu and Brown, Steven P. (2007) Low-load rotor-synchronised Hahn-echo pulse train (RS-HEPT) 1H decoupling in solid-state NMR: factors affecting MAS spin-echo dephasing times. Magnetic Resonance in Chemistry, Vol.45 (No.S1). S198-S208. doi:10.1002/mrc.2145 ISSN 0749-1581.
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Official URL: http://dx.doi.org/10.1002/mrc.2145
Abstract
Transverse dephasing times T-2' in spin-echo MAS NMR using rotor-synchronised Hahn-echo pulse-train (RS-HEPT) low-load H-1 decoupling are evaluated. Experiments were performed at 300 and 600 MHz for (CH)-C-13-labelled L-alanine and (NH)-N-15(delta)-labelled L-histidine center dot HCl center dot H2O, together with SPINEVOLUTION simulations for a ten-spin system representing the crystal structure environment of the (CH)-C-13 carbon in L-alanine. For 30 kHz MAS and nu(1)(H-1) = 100 kHz at 300 MHz, a RS-HEPT T-2' value of 17 +/- 1 ms was obtained for (CH)-C-13-labelled L-alanine which is similar to 50% of the XiX T-2' value of 33 +/- 2 ms. Optimum RS-HEPT decoupling performance is observed for a relative phase of alternate RS-HEPT pi-pulses, Delta phi = phi' - phi, between 40 and 60 degrees. For experiments at 600 MHz and 30 kHz MAS with (CH)-C-13-labelled L-alanine, the best RS-HEPT (nu(1)(H-1) = 100 kHz) T-2' value was 3 times longer than that observed for low-power continuously applied sequences with nu(1)(H-1) <= 40 kHz, i.e. corresponding to the same average power dissipated in the probe. A marked improvement in RS-HEPT H-1 decoupling is observed for increasing MAS frequency: at 55.6 kHz MAS, a best RS-HEPT T-2' value of 34 +/- 5 ms was recorded for (CH)-C-13-labelled L-alanine. Much improved RS-HEPT broadband performance was also observed at 55.6 kHz MAS as compared to 30 kHz MAS. Copyright (c) 2007 John Wiley & Sons, Ltd.
Item Type: | Journal Article | ||||
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Subjects: | Q Science > QD Chemistry Q Science > QC Physics |
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Divisions: | Faculty of Science, Engineering and Medicine > Science > Physics | ||||
Journal or Publication Title: | Magnetic Resonance in Chemistry | ||||
Publisher: | John Wiley & Sons Ltd. | ||||
ISSN: | 0749-1581 | ||||
Official Date: | December 2007 | ||||
Dates: |
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Volume: | Vol.45 | ||||
Number: | No.S1 | ||||
Number of Pages: | 11 | ||||
Page Range: | S198-S208 | ||||
DOI: | 10.1002/mrc.2145 | ||||
Status: | Peer Reviewed | ||||
Publication Status: | Published | ||||
Access rights to Published version: | Restricted or Subscription Access |
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