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同核或異核相關(guān)及自旋為1核的固體核磁共振方法研究

發(fā)布時間:2024-06-02 11:40
  本論文的主要研究目的是開發(fā)固體核磁共振中用于檢測核之間空間相鄰性的同核或異核相關(guān)實驗的新方法。還有一小部分涉及到利用組合脈沖實現(xiàn)氘核的寬帶激發(fā)。第一章簡要地介紹了固體樣品中核自旋的哈密頓相互作用,并詳細介紹了常見的若干同核/異核相關(guān)實驗的方法。在下面的章節(jié)中將會涉及到其中的某些方法,并對這些方法進行了改進。第二章介紹了一種高場條件下的一階(XY8)41超循環(huán)射頻脈沖驅(qū)動重偶實驗(first-order finite-pulse radio-frequency-driven recoupling:fp-RFDR)脈沖序列。這種相位超循環(huán)是通過相位翻轉(zhuǎn)和四量子相循環(huán)來實現(xiàn)的。在高速或者超高速魔角旋轉(zhuǎn)條件下,這種相位超循環(huán)的脈沖方法對以下若干影響因素具有很好的穩(wěn)定性:(i)化學位移各向異性(CSA),(ii)化學位移的差異性,(iii)射頻場的不均勻性,(iv)異核偶極耦合相互作用。我們通過模擬和實驗對比了fp-RFDR-XY8、fp-RFDR-XY16和fp-RFDR-(XY8)41這三種方法在較大的射頻脈沖偏轉(zhuǎn)和強化學位移各項異性作用下的表現(xiàn)。在這些條件下,fp-RFDR-(XY8)41...

【文章頁數(shù)】:181 頁

【學位級別】:博士

【文章目錄】:
摘要
ABSTRACT
Contents
Chapter 1:Introduction
    1.1 Nuclear Spin Interactions in Solids
        1.1.1 Chemical shift and Chemical shift anisotropy
        1.1.2 J-coupling
        1.1.3 Dipolar Coupling
        1.1.4 Quadrupolar interaction
    1.2 Through-space Homo-nuclear Correlation Spectroscopy
        1.2.1 SQ-SQ approach
        1.2.2 DQ-SQ aproach
    1.3 Through-space Hetero-nuclear Correlation Spectroscopy
    References
Chapter 2:Through-space Homo-nuclear Correlation Spectroscopy:fp-RFDR with(XY8)41 super-cycling
    2.1 Pulse sequence
    2.2 Numerical simulations
        2.2.1 Two spin-system
        2.2.2 Three spin-system:choice of rf-field
        2.2.3 Three spin-system:rf-inhomogeneity
        2.2.4 Three spin-system: CSA effect
        2.2.5 CIH-C2H2-H2 spin-system
    2.3 Experimental section
    2.4 Results and Discussion
        2.4.1 13C-13C correlation
        2.4.2 31P-31P correlations
    2.5 Conclusions
    References
Chapter 3:Through-space Homo-nuclear Correlation Spectroscopy:SHANGHAI+
    3.1 Numerical simulations
    3.2 Experimental verifications
    3.3 Conclusion
    References
Chapter 4:Through-space Hetero-nuclear Correlation Spectroscopy:improving theresolution
    4.1 Pulse sequence and theory
        4.1.1 The D-HMQC sequence
        4.1.2 The decoupling sequences
        4.1.3 Time increment optimization
    4.2 Numerical simulations
        4.2.1 Simulation parameters
        4.2.2 Decoupling efficiency
    4.3 Experimental demonstrations
        4.3.1 Sample and experimental conditions
        4.3.2 1H-{13C} D-HMQC 2D experiments at 9.4 T and vR=32.3 kHz
        4.3.3 1H-{13C)D-HMQC 2D experiments at 18.8 T and 21.1 T using vR≈62 kHz
        4.3.4 Application to 1H-{14N} DANTE-D-HMQC at 21.1 T and vR=62.1 kHz
    4.4 Conclusions
    References
Chapter 5:Through-space Hetero-nuclear Correlation Spectroscopy:detection of nucleiexperiencing large anisotropic interactions using frequency-selective pulses
    5.1 Pulse sequence
    5.2 Theory
        5.2.1 Coherence transfer
        5.2.2 Broadband excitation
        5.2.3 Sideband selective excitation
        5.2.4 Excitation of 2Q coherences
    5.3 Numerical simulations
        5.3.1 Simulation parameters
        5.3.2 Simulations for 195Pt nucleus
        5.3.3 Simulations for 14N nucleus
    5.4 Experimental demonstration for 1H-{14N} 1Q-HMQC
        5.4.1 Samples and experimental conditions
        5.4.2 Effect of rf-field and pulse length
        5.4.3 Sensitivity to rotor-synchronization
        5.4.4 Robustness to 14N offset
    5.5 Conclusions
    References
Chapter 6:Revisiting NMR composite pulses for broadband 2H excitation
    6.1 Pulse sequence and its implementation with composite pulse
    6.2 Numerical simulations
    6.3 Experimental
    6.4 Conclusions
    References
Chapter 7:Revisiting NMR composite pulses for broadband 2H excitation:Theoreticalcalculation by average Hamiltonian theory
    7.1 Analytical calculations of COM-Ⅱ
    7.2 Numerical simulations
    7.3 Conclusions
    References
Chapter 8:Resume
Acknowledgements
Curriculum Vitae and Publication



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