Sharma Kshama, Madhu P K, Agarwal Vipin
TIFR Centre for Interdisciplinary Sciences, Tata Institute of Fundamental Research, 21 Brundavan Colony, Narsingi, Hyderabad 500 075, India.
TIFR Centre for Interdisciplinary Sciences, Tata Institute of Fundamental Research, 21 Brundavan Colony, Narsingi, Hyderabad 500 075, India; Department of Chemical Sciences, Tata Institute of Fundamental Research, Homi Bhabha Road, Colaba, Mumbai 400005, India.
J Magn Reson. 2016 Sep;270:136-141. doi: 10.1016/j.jmr.2016.07.007. Epub 2016 Jul 19.
The performance of heteronuclear spin decoupling sequences in solid-state NMR severely degrades when the proton radiofrequency (RF) nutation frequencies (ν1) are close to or at multiples of magic-angle spinning (MAS) frequency (νr) that are referred to as rotary-resonance recoupling conditions (ν1=n·νr). Recently, two schemes, namely, PISSARRO and rCW(ApA), have been shown to be less affected by the problem of MAS and RF interference, specifically at the n=2 rotary-resonance recoupling condition, especially in the fast MAS regime. Here, we systematically evaluate the loss in intensity of several heteronuclear spin decoupling sequences at the n=1, 2 conditions compared to high-power decoupling in the fast-MAS regime. We propose that in the fast-MAS regime (above 40kHz) the entire discussion about RF and MAS interference can be avoided by using appropriate low-power decoupling sequences which give comparable performance to decoupling sequences with high-power (1)H irradiation of ca.195kHz.
当质子射频(RF)章动频率(ν1)接近或为魔角旋转(MAS)频率(νr)的倍数(即所谓的旋转共振重新耦合条件,ν1 = n·νr)时,固态核磁共振中异核自旋去耦序列的性能会严重下降。最近,已证明两种方案,即PISSARRO和rCW(ApA),受MAS和RF干扰问题的影响较小,特别是在n = 2旋转共振重新耦合条件下,尤其是在快速MAS regime中。在这里,我们系统地评估了在快速MAS regime中,与高功率去耦相比,几种异核自旋去耦序列在n = 1、2条件下的强度损失。我们建议,在快速MAS regime(高于40kHz)中,通过使用适当的低功率去耦序列,可以避免关于RF和MAS干扰的整个讨论,这些序列的性能与约195kHz的高功率(1)H照射去耦序列相当。