Max-Planck-Institute of Solid-State Research, Heisenbergstr. 1, 70569 Stuttgart, Germany.
J Magn Reson. 2010 Oct;206(2):255-63. doi: 10.1016/j.jmr.2010.07.018. Epub 2010 Aug 1.
Heteronuclear spin decoupling pulse sequences in solid-state NMR have mostly been designed and applied for irradiating 1H as the abundant nucleus. Here, a systematic comparison of different methods for decoupling 19F in rigid organic solids is presented, with a special emphasis on the recently introduced frequency-swept sequences. An extensive series of NMR experiments at different MAS frequencies was conducted on fluorinated model compounds, in combination with large sets of numerical simulations. From both experiments and simulations it can be concluded that the frequency-swept sequences SWf-TPPM and SWf-SPINAL deliver better and more robust spin decoupling than the original sequences SPINAL and TPPM. Whereas the existence of a large chemical shift anisotropy and isotropic shift dispersion for 19F does compromise the decoupling efficiency, the relative performance hierarchy of the sequences remains unaffected. Therefore, in the context of rigid organic solids under moderate MAS frequencies, the performance trends observed for 19F decoupling are very similar to those observed for 1H decoupling.
固态 NMR 中的异核自旋去耦脉冲序列主要设计和应用于辐照 1H 作为丰富的核。在这里,我们对不同方法在刚性有机固体中对 19F 去耦进行了系统比较,特别强调了最近引入的频率扫描序列。在不同的 MAS 频率下对氟化模型化合物进行了广泛的 NMR 实验,并结合了大量的数值模拟。从实验和模拟中可以得出结论,频率扫描序列 SWf-TPPM 和 SWf-SPINAL 比原始序列 SPINAL 和 TPPM 提供了更好和更稳健的自旋去耦。尽管 19F 的化学位移各向异性和各向同性位移分散很大,但会影响去耦效率,但序列的相对性能层次结构不受影响。因此,在中等 MAS 频率下的刚性有机固体的情况下,观察到的 19F 去耦性能趋势与观察到的 1H 去耦性能趋势非常相似。