Wilcke Sam L, Cairns Elton J, Reimer Jeffrey A
Department of Chemical Engineering, University of California at Berkeley, 201 Gilman Hall, Berkeley, CA 94720, USA.
Solid State Nucl Magn Reson. 2006 Feb;29(1-3):199-203. doi: 10.1016/j.ssnmr.2005.08.001. Epub 2005 Sep 23.
The versatility of using a stochastic pulse sequence to elucidate peaks with a wide range of shifts, peak widths, and T(1) relaxation times is demonstrated. A stochastic sequence is combined with high speed magic angle spinning (MAS) to obtain the broad and largely shifted peak associated with (31)P in LiNiPO(4). A stochastic sequence is also used to obtain a spectrum of 85% H(3)PO(4), which has a much longer T(1) value. The signal-to-noise was comparable for spectra of 85% H(3)PO(4) obtained with either a stochastic sequence or an optimized Ernst angle experiment. Experimental parameters for the stochastic experiment are set depending only on the ringdown of the probe and not on any inherent qualities of the sample. A stochastic sequence, therefore, combined with MAS provides a useful strategy for finding peaks with unknown T(1) relaxation constants, peak widths, and shifts.
本文展示了使用随机脉冲序列来解析具有广泛化学位移、峰宽和T(1)弛豫时间的峰的通用性。将随机序列与高速魔角旋转(MAS)相结合,以获得与LiNiPO(4)中(31)P相关的宽峰且化学位移较大的峰。还使用随机序列来获取85% H(3)PO(4)的谱图,其具有长得多的T(1)值。对于用随机序列或优化的恩斯特角实验获得的85% H(3)PO(4)的谱图,信噪比相当。随机实验的实验参数仅根据探头的衰减来设置,而不取决于样品的任何固有特性。因此,随机序列与MAS相结合为寻找具有未知T(1)弛豫常数、峰宽和化学位移的峰提供了一种有用的策略。