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介绍原理和实验方法

文档名称:介绍原理和实验方法
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文档名称:介绍原理和实验方法
文档关注次数:284
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文档大小:18780KB
上传者:gentianana
添加时间:2017/06/17
内容摘要:
Nuclear Magnetic
Resonance
pectroscopy
An Introduction to Principle
Applications, and Experimental Methods
Joseph B. Lambert
Northwestern University
Eugene P Mazzola
University of Maryland
d
Food and Drug Administration
Joint Institute for Food Safety Applied Nutrition
PEARSON
Prentice
Hall
Pearson Education Inc
pper Saddle River, New Jersey 07458
Contents
Preface xi
1 Introduction 1
1-1 Magnetic Properties of Nuclei 1
1-2 The Chemical Shift 5
1-3 Excitation and Relaxation 8
1-4 Pulsed Experiments 11
1-5 The Coupling Constant 13
1-6 Quantitation and Complex Splitting 19
1-7 Commonly Studied Nuclides 21
1-8 Dynamic Effects 2
1-9 Spectra of Solids 25
oblems
Bibliography 30
2 Introductory Experimental Methods 31
2-1 The Spectrometer 31
2-2 Sample Preparation 33
2-3O
ag the Signal
2-3a Sample Tube Placement 34
2-3b Probe Adjustment
2-3c Field/Frequency Locking 35
2-3d Spectrometer Shimming 36
2-4 Determination of NMR Spectra: Acquisition Parameters 39
2-4a Number of Data Points 4
2-4b Spectral Width 4
2-4c Filter Bandwidth 42
2-4d Acquisition Time 42
2-4e Transmitter Offset 43
2-4f Flip Angle 43
4g Receiver Gain 45
2-4h Number of Scans 45
2-4i Steady-state Scans 46
2-4j Oversampling and Digital Filtration 46
-4k Decoupling for X Nuclei 46
2-41 Typical NMR Experiments 47
2-5 Determination of NMR Spectra: Processing Parameters 48
Sa Exponential Weighting 4s
2-5b Zero Filling 49
2-5C FID Truncation and Spectral Artifacts 50
2-5d Resolution 5I
2-6 Determination of NMR Spectra: Spectral Presentation 52
2-6a Signal Phasing and Baseline Correction 52
2-6b Zero Referencing 55
2-6c Determination of Certain NMR Parameters 56
2-7 Calibr
2-7a Pulse Width (Flip Angle) 58
b Decoupler Field Strength 60
Bibliography 6
3 The Chemical Shift 62
3-1 Factors that Infl
Proton Shifts 6
3-2 Proton Chemical Shifts and Structure 69
3-2a Saturated Aliphatics 69
3-2b Unsaturated Aliphatics 71
3-2c Aromatics 73
nd Nit
3-2e Programs for Empirical Calculations 76
3-3 Medium and Isotope Effects 76
3-4 Factors that Influence Carbon Shifts 79
3-5 Carbon Chemical Shifts and Structure 81
3-5a Saturated Aliphatics 82
3-5b Unsaturated Compounds 86
s88
3-5d Programs for Empirical Calculation 88
3-6 Tables of Chemical Shifts 8
Problems 9I
Bibliography 97
4 The Coupling Constant 98
4-1 First- and Second-order Spectra 98
4-2 Chemical and Magnetic Equivalence 99
4-3 Signs and Mechanisms: One-bond Couplings 104
4-4 Geminal Couplings
4-5V
couplings
4-6 Long-range Couplings 112
4-7 Spectral Analysis 115
4-8 Tables of Coupling Constants 119
12
Bibliography 129
5 Further Topics in One-dimensional NMR 131
5-1 Spin-lattice and Spin-spin Relaxation 131
5-2 Reactions on the NMR Time Scale 36
5-3 Multiple Resonance 143
5-4 The Nuclear Overhauser Effect 48
Editing 153
5-6 Sensitivity Enhancement 156
5-7 Carbon Connectivity 162
5-8 Phase Cycling, Composite Pulses, and Shaped Pulses 163
Problems 166
Bibliography 170
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