固体核磁共振异核相关新脉冲的开发及同核相关数据处理新方法

发布时间：2021-08-25 13:46

　　本论文主要关注于固体核磁共振的研宄,包括异核相关实验新方法的开发和同核相关实验的数据处理新方法。在第一章中,我们简要回顾了核磁共振的发展历史。在1945年,以Bloch和Pmcell为首的两个实验小组同时发现了核磁共振现象,并于1952年获得诺贝尔物理学奖,在随后的几十年里,高磁场、高转速以及各种脉冲序列技术快速发展、不断进步,时至今日已成为分析分子结构和研宄化学动力的重要手段,在有机化学、生物化学和药物化学等领域里得到了广泛的应用。其次,我们简要阐述了核磁共振中涉及的各种相互作用及其哈密顿量。核磁共振谱会受到来自外部仪器和样品内部的多种相互作用的影响,前者称为外部相互作用,后者称为内部相互作用。外部相互作用主要由外磁场,射频场和梯虔场引起。内部相互作用包括化学位移各向异性、偶极-偶极相互作用、J偶合相互作用和四级相互作用（只对于自旋量子数大于1/2的核）。我们给出了这些相互作用的解释及其哈密顿量。再次,我们介绍了一种及其重要的技术,即改变四级核能级布居数。因在所有核磁共振可检测核中,四级核约占70%,灵敏度依然是四级核核磁共振的中心问题。我们主要介绍了三种形状脉冲的原理:WURST（... 

【文章来源】：华东师范大学上海市 211工程院校 985工程院校 教育部直属院校

【文章页数】：104 页

【学位级别】：博士

【文章目录】：
中文摘要
Abstract
Chapter 1:Introduction
    1.1. History of Solid State NMR
    1.2. Hamiltonians and their manipulations
        1.2.1 The external spin interactions
        1.2.2 The internal spin interactions
    1.3 Population transfer from satellite transitions
        1.3.1 WURST
        1.3.2 DFS
        1.3.3 HS
    1.4. NMR Spectrum
        1.4.1 Fourier transformation two-dimensional (FT2D)spectroscopy
        1.4.2 Covariance Spectroscopy
    1.5. New strategy
        1.5.1 PT-HMQC
        1.5.2 COV2D combined with various sampling schemes and accumulation profiles
    References
Chapter 2:New pulse sequence for heteronuclear experiments
    2.1 Theory
        2.1.1 Indirect detection of quadrupolar nuclei using J-HMQC
        2.1.2 Indirect detection of quadrupolar nuclei using PT-J-HMQC
    2.2 Simulations and Experiments of PT-HMQC
        2.2.1 Simulations
        2.2.2 Experiments
            2.2.2.1 ~(31)P-{~(27)Al}PT-J-HMQC on AlPO_4-HAD and Mu-4 sample
            2.2.2.2 PT-J-HMQC for two half-integer quadrupolar species on Al_2O_3 sample
            2.2.2.3 ~(31)P-{~(27)Al}PT-D-HMQC on APO_4-14 sample
    2.3 Improve Methods of PT-J-HMQC
        2.3.1 Simulations
            2.3.1.1 Double sweeps pulse
            2.3.1.2 Quadruple sweeps pulse
        2.3.2 Experiments
            2.3.2.1 Experiments for Berlinite
            2.3.2.2 Experiments for AlPO_4-14
    2.4 Conclusion
    References
Chapter 3:New data processing methods for homonuclear experiments
    3.1 covariance spectroscopy with a non-uniform continuous acquisition scheme forsignal enhancement
        3.1.1 Background
            3.1.1.1 Conventional UCA-FT2D spectroscopy
            3.1.1.2 Profiles for Non-Uniform Continuous Acquisition schemes
        3.1.2 Experimental section
        3.1.3 Results and discussion
        3.1.4 Conclusion
    3.2 Comparison of various sampling schemes and accumulation profiles in covariance spectroscopy with exponentially decaying 2D signals
        3.2.1 Background
            3.2.1.1 Conventional US-FT2D spectroscopy
            3.2.1.2 Gaussian accumulation profile
            3.2.1.3 CUO and NUS restricted sampling schemes
            3.2.1.4 Covariance spectroscopy
            3.2.1.5 Noise with covariance treatment
        3.2.2 Results and discussion
            3.2.2.1 Comparison of various S/N_(peak-ridge) and S/N_(peak-free)
            3.2.2.2 Constant time S/N_(peak-ridge) and S/N_(peak-free)
            3.2.2.3 Set up of the covariance acquisition
            3.2.2.4 Application of covariance to[U-~(13)C,~(15)N]-proteo-rhodopsin
        3.2.3 Conclusion
    References
Resume
Acknowledgements
Paper List



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