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Article Dans Une Revue Journal of Chemical Physics Année : 2022

Heteronuclear decoupling with rotor-synchronized phase-alternated cycles

Résumé

A new heteronuclear decoupling pulse sequence is introduced, dubbed ROtor-Synchronized Phase-Alternated Cycles (ROSPAC). It is based on a partial refocusing of the coherences (spin operator products or cross-terms) [Filip et al., J. Mag. Reson. 176, 2 (2005)] responsible for transverse spin-polarization dephasing, on the irradiation of a large pattern of radio-frequencies, and on a significant minimization of the cross-effects implying 1 H chemical-shift anisotropy. Decoupling efficiency is analyzed by numerical simulations and experiments and compared to that of established decoupling sequences [swept-frequency two-pulse phase-modulated (TPPM), TPPM, small phase incremental alternation (SPINAL), refocused Continuous-wave (CW Apa ), and Rotor-Synchronized Hahn-Echo pulse train (RS-HEPT)]. It was found that ROSPAC offers good 1 H offset robustness for a large range of chemical shifts and low radio-frequency (RF) powers, and performs very well in the ultra-fast magic-angle spinning (MAS) regime, where it is almost independent from RF power and permits it to avoid rotary-resonance recoupling conditions ( v 1 = nv r , n = 1, 2). It has the advantage that only the pulse lengths require optimization and has a low duty cycle in the pulsed decoupling regime. The efficiency of the decoupling sequence is demonstrated on a model microcrystalline sample of the model protein domain GB 1 at 100 kHz MAS at 18.8 T.
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Dates et versions

hal-03852887 , version 1 (15-11-2022)

Identifiants

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Andrea Simion, Tobias Schubeis, Tanguy Le Marchand, Mihai Vasilescu, Guido Pintacuda, et al.. Heteronuclear decoupling with rotor-synchronized phase-alternated cycles. Journal of Chemical Physics, 2022, 157 (1), pp.014202. ⟨10.1063/5.0098135⟩. ⟨hal-03852887⟩
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