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天然高分子材料的超高分辨率¹H 固体核磁共振

Very high-resolution 1H MAS NMR of a natural polymeric material.

作者信息

Gil A M, Lopes M H, Neto C P, Rocha J

机构信息

Department of Chemistry, University of Aveiro, Portugal.

出版信息

Solid State Nucl Magn Reson. 1999 Oct;15(1):59-67. doi: 10.1016/s0926-2040(99)00047-8.

Abstract

The use of ultrafast magic angle spinning (> 30 kHz) in tandem with delayed echo acquisition is shown to yield very high-resolution lH MAS NMR spectra of complex natural organic materials. For the first time, very high-resolution 1H MAS NMR spectra are reported for cork and wood components, two natural materials with great economic importance. The effect of the spinning rate on the 1H NMR spectra was evaluated with single-pulse acquisition and delayed-echo acquisition. The delayed-echo acquisition spectra presented linewidths as sharp as 67 and 25 Hz. The narrow peaks, characterised by proton spin-spin and spin-lattice relaxation, were assigned to the isotropic chemical shifts and the general spectral features were shown to correlate with the sample chemical structure. The tentative assignments of cork 1H MAS NMR signals were presented.

摘要

超快速魔角旋转(> 30 kHz)与延迟回波采集相结合,已被证明可产生复杂天然有机材料的高分辨率1H MAS NMR光谱。首次报道了软木和木材成分这两种具有重要经济意义的天然材料的高分辨率1H MAS NMR光谱。通过单脉冲采集和延迟回波采集评估了旋转速率对1H NMR光谱的影响。延迟回波采集光谱的线宽锐至67和25 Hz。由质子自旋-自旋和自旋-晶格弛豫表征的窄峰被指定为各向同性化学位移,并且显示出一般光谱特征与样品化学结构相关。给出了软木1H MAS NMR信号的初步归属。

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