Efficient rotational echo double resonance recoupling of a spin-1/2 and a quadrupolar spin at high spinning rates and weak irradiation fields

A modification of the rotational echo (adiabatic passage) double resonance experiments, which allows recoupling of the dipolar interaction between a spin-1/2 and a half integer quadrupolar spin is proposed. We demonstrate efficient and uniform recoupling at high spinning rates (νr), low radio-frequency (RF) irradiation fields (ν1), and high values of the quadrupolar interaction (νq) that correspond to values of α =ν12/νqνr, the adiabaticity parameter, which are down to less than 10% of the traditional adiabaticity limit for a spin-5/2 (α = 0.55). The low-alpha rotational echo double resonance curve is obtained when the pulse on the quadrupolar nucleus is extended to full two rotor periods and beyond. For protons (spin-1/2) and aluminum (spin-5/2) species in the zeolite SAPO-42, a dephasing curve, which is significantly better than the regular REAPDOR experiment (pulse length of one-third of the rotor period) is obtained for a spinning rate of 13 kHz and RF fields down to 10 and even 6 kHz. Under these conditions, α is estimated to be approximately 0.05 based on an average quadrupolar coupling in zeolites. Extensive simulations support our observations suggesting the method to be robust under a large range of experimental values.