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Low-power 14N decoupling at fast MAS of 70 kHz
Ekta Nehra1, Vipin Agarwal2, Yusuke Nishiyama1
1JEOL Ltd., Akishima, Tokyo, 196-8558, Japan.
Abstract:
Higher isotropic resolution in solids is essential for accurate assignment of the chemical shifts in multisite chemical and biological systems; consequently, the pursuit of solution-like resolution in solid samples remains an ongoing challenge. MAS provides the effective averaging of the anisotropic interactions to the first-order while the higher order interactions, such as residual dipolar splitting (RDS), and isotropic interactions like J coupling remain. With the emergence of faster MAS, RDS and J couplings become significant constraints in the resolution and sensitivity of isotropic 1H peaks bonded to 14N. However, the dominant quadrupolar coupling hampers the decoupling of 1H-14N, since the achievable 14N RF-field strength is much smaller than the size of the quadrupolar coupling. Therefore, 14N edited spectroscopy is typically performed in the absence of 14N decoupling, leading to broader 1H linewidth and reduced sensitivity. In this context, we propose the continuous-wave (CW) 14N decoupling of 14N-1H spin pair under 1H detection at a fast MAS of 70 kHz. We experimentally show that the on-resonance low-power 14N CW irradiation at fast MAS yields the narrower linewidth. Utilizing the quadrupolar jolting frame description, a qualitative analysis of the optimum decoupling effect is provided.
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