Das Bibhuti B, Sinha N, Ramanathan K V
Department of Physics, Indian Institute of Science, Bangalore, India.
J Magn Reson. 2008 Oct;194(2):237-44. doi: 10.1016/j.jmr.2008.07.010. Epub 2008 Jul 17.
The measurement of hetero-nuclear dipolar coupling using two-dimensional separated local field (SLF-2D) NMR experiments is a powerful technique for the determination of the structure and dynamics of molecules in the solid state and in liquid crystals. However, the experiment is sensitive to a number of factors such as the Hartmann-Hahn match condition, proton frequency off-set and rf heating. It is shown here that by the use of phase alternated pulses during spin-exchange the effect of rf mismatch on the dipolar coupling measurement can be compensated over a wide range of off-sets. Phase alternation together with time and amplitude modulation has also been considered and incorporated into a pulse scheme that combines spin exchange with homonuclear spin decoupling based on magic sandwich sequence and named as SAMPI4. Such time and amplitude averaged nutation experiments use relatively low rf power and generate less sample heating. One of these schemes has been applied on liquid crystal samples and is observed to perform well and yield spectra with high resolution.
使用二维分离局部场(SLF - 2D)核磁共振实验测量异核偶极耦合是一种用于确定固态和液晶中分子结构与动力学的强大技术。然而,该实验对许多因素敏感,如哈特曼 - 哈恩匹配条件、质子频率偏移和射频加热。本文表明,通过在自旋交换期间使用相位交替脉冲,射频失配对偶极耦合测量的影响可以在很宽的偏移范围内得到补偿。相位交替以及时间和幅度调制也已被考虑并纳入一种脉冲序列,该序列基于魔术三明治序列将自旋交换与同核自旋去耦相结合,命名为SAMPI4。这种时间和幅度平均的章动实验使用相对较低的射频功率,产生的样品加热较少。这些方案之一已应用于液晶样品,观察到其性能良好并能产生高分辨率光谱。