Effects of insufficient 31P pulse amplitudes on 13C-detected 31P13C rotational-echo double-resonance measurements in solid state NMR

IF 1.9 3区化学 Q3 BIOCHEMICAL RESEARCH METHODS

Journal of magnetic resonance Pub Date : 2025-05-28 DOI:10.1016/j.jmr.2025.107908

Motahareh G. Larimi, Robert Tycko

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Abstract

We investigate the effects of insufficient ³¹P pulse amplitudes on ¹³C-detected ³¹P¹³C Rotational-Echo Double-Resonance (REDOR) measurements in a 17.5 T magnetic field. Experimental REDOR data on two compounds show that normalized REDOR difference signals

Δ S / S_{0}

are suppressed when the amplitudes of ³¹P π pulse trains are not very large compared with the ³¹P chemical shift anisotropies. This behavior is explained theoretically by an analysis of the effects of imperfections in π pulse rotations due to the orientation-dependent and time-dependent resonance offsets under magic-angle spinning in REDOR measurements. We show that effects of the same pulse imperfections can be observed directly by measurements of an effective relaxation time

{T_{1}}^{eff}

for longitudinal ³¹P spin polarization under identical π pulse trains.

Abstract Image

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固态核磁共振中31P脉冲幅值不足对13c检测31P13C旋转回波双共振测量的影响

我们研究了在17.5 T磁场中，31P脉冲幅度不足对13c探测到的31P13C旋转回波双共振（REDOR）测量的影响。两种化合物的实验REDOR数据表明，当31P π脉冲序列的幅度不是很大时，归一化REDOR差分信号ΔS/S0被抑制。从理论上解释了这种行为，分析了在REDOR测量中，由于魔角旋转下的方向相关和时间相关的共振偏移，π脉冲旋转中的缺陷的影响。通过测量相同π脉冲序列下纵向31P自旋极化的有效弛豫时间T1eff，可以直接观察到相同脉冲缺陷的影响。

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来源期刊

Journal of magnetic resonance 物理-光谱学

CiteScore

3.80

自引率

13.60%

发文量

150

审稿时长

69 days

期刊介绍： The Journal of Magnetic Resonance presents original technical and scientific papers in all aspects of magnetic resonance, including nuclear magnetic resonance spectroscopy (NMR) of solids and liquids, electron spin/paramagnetic resonance (EPR), in vivo magnetic resonance imaging (MRI) and spectroscopy (MRS), nuclear quadrupole resonance (NQR) and magnetic resonance phenomena at nearly zero fields or in combination with optics. The Journal''s main aims include deepening the physical principles underlying all these spectroscopies, publishing significant theoretical and experimental results leading to spectral and spatial progress in these areas, and opening new MR-based applications in chemistry, biology and medicine. The Journal also seeks descriptions of novel apparatuses, new experimental protocols, and new procedures of data analysis and interpretation - including computational and quantum-mechanical methods - capable of advancing MR spectroscopy and imaging.