Department of Chemistry, Berea College, Berea, KY 40404, USA.
J Magn Reson. 2011 Jan;208(1):70-5. doi: 10.1016/j.jmr.2010.10.006. Epub 2010 Oct 29.
The primary shortcoming of the z-filtered refocused INADEQUATE MAS NMR pulse sequence is the possibility of artifacts introduced during the z-filter due to spin diffusion where by extra peaks in the single-quantum dimension (from other sites in the molecule) appear correlated with a given double-quantum frequency. This is a problem when the spinning speeds are too slow (less than 15 kHz) to sufficiently average the proton-proton homonuclear dipolar couplings. This would be especially important when working with large volume rotors that are difficult to spin fast enough to completely average the homonuclear couplings. In our experiments we used the frequency-switched Lee-Goldberg (FSLG) method of homonuclear decoupling during the z-filter to remove the artifact peaks. This method has the advantage of being quite easy to setup and implement on most modern NMR spectrometers.
z 滤波再聚焦 INADEQUATE MAS NMR 脉冲序列的主要缺点是,由于自旋扩散,在 z 滤波过程中可能会引入伪影,从而导致单量子维度(来自分子中的其他位置)中的额外峰与给定的双量子频率相关。当旋转速度太慢(小于 15 kHz)以至于不能充分平均质子-质子同核偶极耦合时,这就是一个问题。当处理难以旋转得足够快以完全平均同核偶极耦合的大容量转子时,这将尤为重要。在我们的实验中,我们在 z 滤波期间使用了 Lee-Goldberg 频移(FSLG)方法来消除伪影峰。这种方法的优点是在大多数现代 NMR 光谱仪上非常容易设置和实现。