Preprints
https://doi.org/10.5194/mr-2024-13
https://doi.org/10.5194/mr-2024-13
02 Sep 2024
 | 02 Sep 2024
Status: a revised version of this preprint was accepted for the journal MR and is expected to appear here in due course.

Low-Power WALTZ Decoupling under Magic-Angle Spinning

Luzian Thomas and Matthias Ernst

Abstract. Heteronuclear low-power decoupling using the solution-state WALTZ sequences has become quite popular in solid-state protein NMR and seems to work well. However, there are no systematic studies that characterize these sequences under magic-angle spinning (MAS) and give recommendations which parameter should be used. We have studied in detail the use of WALTZ-16 and WALTZ-64 as low-power decoupling sequences under 100 kHz MAS by characterizing the resonance conditions analytically, using numerical simulations, and experiments on model substances. The recoupling at heteronuclear resonance conditions between the modulation frequency of the sequences and the MAS frequency is the most important feature. Pulse lengths corresponding to areas with vanishing first-order heteronuclear recoupling are good candidates for efficient decoupling. We have characterized two such conditions defined by ν1r/10 or τ90r/4 and ν1=2 νr/5 or τ90r which both lead to narrow lines and are stable against rf-field variations and chemical-shift offsets. More such conditions might exist but were not investigated here.

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Luzian Thomas and Matthias Ernst

Status: closed

Comment types: AC – author | RC – referee | CC – community | EC – editor | CEC – chief editor | : Report abuse
  • RC1: 'Comment on mr-2024-13', Anonymous Referee #1, 12 Sep 2024
    • AC1: 'Reply on RC1', Matthias Ernst, 12 Sep 2024
  • RC2: 'Comment on mr-2024-13', Anonymous Referee #2, 18 Sep 2024
    • AC2: 'Reply on RC2', Matthias Ernst, 19 Sep 2024

Status: closed

Comment types: AC – author | RC – referee | CC – community | EC – editor | CEC – chief editor | : Report abuse
  • RC1: 'Comment on mr-2024-13', Anonymous Referee #1, 12 Sep 2024
    • AC1: 'Reply on RC1', Matthias Ernst, 12 Sep 2024
  • RC2: 'Comment on mr-2024-13', Anonymous Referee #2, 18 Sep 2024
    • AC2: 'Reply on RC2', Matthias Ernst, 19 Sep 2024
Luzian Thomas and Matthias Ernst
Luzian Thomas and Matthias Ernst

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Short summary
The paper investigates the suitability of an existing solution-state NMR spin decoupling sequence for use as a low-power solid-state NMR decoupling sequence under sample spinning. Complications arise from resonance conditions between the spin modulations by the pulse sequence and the sample rotation. We show that the timing of the pulse sequence is the most important criterion to achieve good decoupling. The paper gives recommendations for optimum parameters.