Department of Chemistry, Ohio State University, 100 West 18th Avenue, Columbus, Ohio 43210, USA.
J Chem Phys. 2013 May 7;138(17):174203. doi: 10.1063/1.4803142.
A general approach for enhancing sensitivity of nuclear magnetic resonance sideband separation experiments, such as Two-Dimensional One Pulse (TOP), Magic-Angle Turning (MAT), and Phase Adjust Spinning Sidebands (PASS) experiments, with phase incremented echo-train acquisition (PIETA) is described. This approach is applicable whenever strong inhomogeneous broadenings dominate the unmodulated frequency resonances, such as in non-crystalline solids or in samples with large residual frequency anisotropy. PIETA provides significant sensitivity enhancements while also eliminating spectral artifacts would normally be present with Carr-Purcell-Meiboom-Gill acquisition. Additionally, an intuitive approach is presented for designing and processing echo train acquisition magnetic resonance experiments on rotating samples. Affine transformations are used to relate the two-dimensional signals acquired in TOP, MAT, and PASS experiments to a common coordinate system. Depending on sequence design and acquisition conditions two significant artifacts can arise from truncated acquisition time and discontinuous damping in the T2 decay. Here we show that the former artifact can always be eliminated through selection of a suitable affine transformation, and give the conditions in which the latter can be minimized or removed entirely.
描述了一种增强核磁共振边带分离实验(如二维单脉冲(TOP)、魔角旋转(MAT)和相调旋转边带(PASS)实验)灵敏度的通用方法,该方法结合了相位递增回波串采集(PIETA)。只要强非均匀展宽主导未调制频率共振,例如非晶固体或具有较大残余频率各向异性的样品,该方法都是适用的。PIETA 提供了显著的灵敏度增强,同时消除了 Carr-Purcell-Meiboom-Gill 采集通常会出现的光谱伪影。此外,还提出了一种直观的方法来设计和处理旋转样品上的回波串采集磁共振实验。仿射变换用于将在 TOP、MAT 和 PASS 实验中采集的二维信号与公共坐标系相关联。根据序列设计和采集条件,截断采集时间和 T2 衰减中的不连续阻尼会产生两个显著的伪影。这里我们表明,通过选择合适的仿射变换,可以消除前一个伪影,并给出了后一个伪影可以最小化或完全消除的条件。