波谱学杂志 ›› 2020, Vol. 37 ›› Issue (1): 1-15.doi: 10.11938/cjmr20192779

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固体核磁共振魔角旋转条件下的定量交叉极化技术(英文)

梁力鑫1,3, 邓风2, 侯广进1   

  1. 1. 催化基础国家重点实验室, 洁净能源国家实验室, 能源材料化学协同创新中心, 中国科学院 大连化学物理研究所, 辽宁 大连 116023;
    2. 波谱与原子分子物理国家重点实验室, 武汉磁共振中心(中国科学院 武汉物理与数学研究所), 湖北 武汉 430071;
    3. 中国科学院大学, 北京 100049
  • 收稿日期:2019-08-29 出版日期:2020-03-05 发布日期:2019-10-16
  • 通讯作者: 侯广进,Tel:0411-82463021,E-mail:ghou@dicp.ac.cn;邓风,Tel:027-87198820,E-mail:dengf@wipm.ac.cn. E-mail:ghou@dicp.ac.cn;dengf@wipm.ac.cn
  • 基金资助:
    the National Natural Science Foundation of China (21773230); Liaoning Revitalization Talents Program (XLYC1807207); Innovation Foundation of Dalian Institute of Chemical Physics (Y7611105T5).

Quantitative Cross Polarization Magic-Angle Spinning NMR Spectroscopy in Solids

LIANG Li-xin1,3, DENG Feng2, HOU Guang-jin1   

  1. 1. State Key Laboratory of Catalysis, National Laboratory for Clean Energy, Collaborative Innovation Center of Chemistry for Energy Materials, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, China;
    2. State Key Laboratory of Magnetic Resonance and Atomic and Molecular Physics, National Center for Magnetic Resonance in Wuhan(Wuhan Institute of Physics and Mathematics, Chinese Academy of Sciences), Wuhan 430071, China;
    3. University of Chinese Academy of Sciences, Beijing 100049, China
  • Received:2019-08-29 Online:2020-03-05 Published:2019-10-16
  • Supported by:
    the National Natural Science Foundation of China (21773230); Liaoning Revitalization Talents Program (XLYC1807207); Innovation Foundation of Dalian Institute of Chemical Physics (Y7611105T5).

摘要: 交叉极化与魔角旋转结合(CP/MAS)的方法已经成为增强固体核磁共振(NMR)检测灵敏度最重要的技术之一.CP/MAS技术的应用大大提高了固体NMR谱图的采集效率.然而,I-S偶极耦合作用、旋转坐标系下的自旋-晶格弛豫、分子运动,以及样品中丰核的分布情况等因素,通常会导致CP/MAS谱图失去定量作用.近年来,多个研究组通过改进或者设计新型固体NMR脉冲序列,获得了基于CP的可用于定量分析的固体NMR谱图.本综述首先简要介绍了CP及CP动力学,随后介绍了一系列基于CP的定量固体NMR信号增强技术,具体包括ramped-amplitude CP(RAMP-CP)、multiple-contact CP、quantification of CP(QCP)、Lee-Goldburg frequency modulated CP(LG-FMCP)和quantitative CP(QUCP).

关键词: 固体核磁共振, 定量核磁共振, 定量交叉极化, 弛豫时间

Abstract: The combination of cross polarization and magic-angle spinning (CP/MAS), is a routine technique for signal enhancement in solid-state nuclear magnetic resonance (NMR) spectrum. With CP/MAS, the acquisition efficiency of solid-state NMR experiments can be improved greatly. However, the enhanced signal is not quantitative according to the different CP dynamics dominated by several factors including heteronuclear dipolar couplings, spin-lattice relaxation times in the rotating frame, molecular motions, number of around abundant spins, and so on. Over the years, numerous efforts have been made to obtain quantitative CP/MAS spectroscopy. This review firstly briefly illustrated the introduction of CP and CP dynamics, and then a series of quantitative NMR methods based on CP were introduced, including ramped-amplitude CP (RAMP-CP), multiple-contact CP, quantification of CP (QCP), Lee-Goldburg frequency modulated CP (LG-FMCP) and quantitative CP (QUCP).

Key words: solid state NMR, quantitative NMR, quantitative cross polarization, relaxation time

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