Nuclear magnetic resonance spectroscopy : an introduction to principles, applications, and experimental methods /: an introduction to principles, applications, and experimental methods. (2018)

• Record Type: Book
• Further Information: Note: Joseph B. Lambert, Eugene Mazzola, Clark D. Ridge.
• Authors: Lambert, Joseph B; Mazzola, Eugene P; Ridge, Clark, 1980-
• Contents: Preface to First Edition xiii Acknowledgments xiv Preface to Second Edition xv Acknowledgments xvi Solutions xvii Symbols xix Abbreviations xxi 1 Introduction 1 1.1 Magnetic Properties of Nuclei 1 1.2 The Chemical Shift 6 1.3 Excitation and Relaxation 10 1.4 Pulsed Experiments 13 1.5 The Coupling Constant 16 1.6 Quantitation and Complex Splitting 23 1.7 Commonly Studied Nuclides 25 1.8 Dynamic Effects 28 1.9 Spectra of Solids 30 Problems 33 Tips on Solving NMR Problems 36 References 37 Further Reading 38 2 Introductory ExperimentalMethods 39 2.1 The Spectrometer 39 2.2 Sample Preparation 41 2.3 Optimizing the Signal 42 2.3.1 Sample Tube Placement 42 2.3.2 Probe Tuning 43 2.3.3 Field/Frequency Locking 43 2.3.4 Spectrometer Shimming 44 2.4 Determination of NMR Spectral-Acquisition Parameters 48 2.4.1 Number of Data Points 50 2.4.2 SpectralWidth 50 2.4.3 Filter Bandwidth 52 2.4.4 Acquisition Time 52 2.4.5 Transmitter Offset 52 2.4.6 Flip Angle 52 2.4.7 Receiver Gain 54 2.4.8 Number of Scans 55 2.4.9 Steady-State Scans 55 2.4.10 Oversampling and Digital Filtration 56 2.4.11 Decoupling for X Nuclei 56 2.4.12 Typical NMR Experiments 57 2.5 Determination of NMR Spectral-Processing Parameters 58 2.5.1 ExponentialWeighting 59 2.5.2 Zero Filling 59 2.5.3 FID Truncation and Spectral Artifacts 60 2.5.4 Resolution 62 2.6 Determination of NMR Spectra: Spectral Presentation 63 2.6.1 Signal Phasing and Baseline Correction 63 2.6.2 Zero Referencing 66 2.6.3 Determination of Certain NMR Parameters 66 2.6.3.1 Chemical Shifts and Coupling Constants 66 2.6.3.2 1H Integration 68 2.7 Calibrations 70 2.7.1 PulseWidth (Flip Angle) 70 2.7.2 Decoupler Field Strength 72 Problems 73 References 74 Further Reading 74 3 The Chemical Shift 75 3.1 Factors That Influence Proton Shifts 75 3.1.1 Local Fields 75 3.1.2 Nonlocal Fields 77 3.2 Proton Chemical Shifts and Structure 85 3.2.1 Saturated Aliphatics 85 3.2.1.1 Alkanes 85 3.2.1.2 Functionalized Alkanes 86 3.2.2 Unsaturated Aliphatics 87 3.2.2.1 Alkynes 87 3.2.2.2 Alkenes 88 3.2.2.3 Aldehydes 89 3.2.3 Aromatics 89 3.2.4 Protons on Oxygen and Nitrogen 90 3.2.5 Programs for Empirical Calculations 91 3.3 Medium and Isotope Effects 92 3.3.1 Medium Effects 92 3.3.2 Isotope Effects 95 3.4 Factors That Influence Carbon Shifts 96 3.5 Carbon Chemical Shifts and Structure 98 3.5.1 Saturated Aliphatics 98 3.5.1.1 Acyclic Alkanes 98 3.5.1.2 Cyclic Alkanes 101 3.5.1.3 Functionalized Alkanes 101 3.5.2 Unsaturated Compounds 103 3.5.2.1 Alkenes 103 3.5.2.2 Alkynes and Nitriles 104 3.5.2.3 Aromatics 104 3.5.3 Carbonyl Groups 105 3.5.4 Programs for Empirical Calculations 105 3.6 Tables of Chemical Shifts 106 Problems 110 Further Tips on Solving NMR Problems 119 References 122 Further Reading 122 4 The Coupling Constant 125 4.1 First- and Second-order Spectra 125 4.2 Chemical and Magnetic Equivalence 126 4.3 Signs and Mechanisms of Coupling 132 4.4 Couplings over One Bond 134 4.5 Geminal Couplings 136 4.6 Vicinal Couplings 139 4.7 Long-range Couplings 143 4.7.1 σ–π Overlap 143 4.7.2 Zigzag Pathways 144 4.7.3 Through-Space Coupling 145 4.8 Spectral Analysis 146 4.9 Second-order Spectra 147 4.9.1 Deceptive Simplicity 147 4.9.2 Virtual Coupling 149 4.9.3 Shift Reagents 150 4.9.4 Isotope Satellites 150 4.10 Tables of Coupling Constants 151 Problems 157 References 169 Further Reading 170 5 Further Topics in One-Dimensional NMR Spectroscopy 173 5.1 Spin–Lattice and Spin–Spin Relaxation 173 5.1.1 Causes of Relaxation 173 5.1.2 Measurement of Relaxation Time 175 5.1.3 Transverse Relaxation 176 5.1.4 Structural Ramifications 177 5.1.5 Anisotropic Motion 177 5.1.6 SegmentalMotion 178 5.1.7 Partially Relaxed Spectra 178 5.1.8 Quadrupolar Relaxation 178 5.2 Reactions on the NMR Time Scale 180 5.2.1 Hindered Rotation 181 5.2.2 Ring Reversal 183 5.2.3 Atomic Inversion 183 5.2.4 Valence Tautomerizations and Bond Shifts 185 5.2.5 Quantification 187 5.2.6 Magnetization Transfer and Spin Locking 187 5.3 Multiple Resonance 188 5.3.1 Spin Decoupling 188 5.3.2 Difference Decoupling 190 5.3.3 Classes of Multiple Resonance Experiments 190 5.3.4 Off-resonance Decoupling 191 5.4 The Nuclear Overhauser Effect 194 5.4.1 Origin 194 5.4.2 Observation 195 5.4.3 Difference NOE 198 5.4.4 Applications 199 5.4.5 Limitations 200 5.5 Spectral Editing 200 5.5.1 The Spin–Echo Experiment 201 5.5.2 The Attached Proton Test 201 5.5.3 The DEPT Sequence 204 5.6 Sensitivity Enhancement 205 5.6.1 The INEPT sequence 206 5.6.2 Refocused INEPT 208 5.6.3 Spectral Editing with Refocused INEPT 208 5.6.4 DEPT Revisited 210 5.7 Carbon Connectivity 212 5.8 Phase Cycling, Composite Pulses, and Shaped Pulses 213 5.8.1 Phase Cycling 213 5.8.2 Composite Pulses 215 5.8.3 Shaped Pulses 215 Problems 217 References 231 Further Reading 231 6 Two-Dimensional NMR Spectroscopy 237 6.1 Proton–Proton CorrelationThrough J Coupling 237 6.1.1 COSY45 247 6.1.2 Long-Range COSY (LRCOSY or Delayed COSY) 248 6.1.3 Phase-Sensitive COSY (ϕ-COSY) 249 6.1.4 Multiple Quantum Filtration 250 6.1.5 TOtal Correlation SpectroscopY (TOCSY) 252 6.1.6 Relayed COSY 252 6.1.7 J-Resolved Spectroscopy 252 6.1.8 COSY for Other Nuclides 254 6.2 Proton–Heteronucleus Correlation 254 6.2.1 HETCOR 255 6.2.2 HMQC 257 6.2.3 BIRD-HMQC 257 6.2.4 HSQC 260 6.2.5 COLOC 260 6.2.6 HMBC 260 6.2.7 Heteronuclear Relay Coherence Transfer 263 6.3 Proton–Proton CorrelationThrough Space or Chemical Exchange 264 6.4 Carbon–Carbon Correlation 268 6.5 Higher Dimensions 270 6.6 Pulsed Field Gradients 273 6.7 Diffusion-Ordered Spectroscopy 277 6.8 Summary of 2D Methods 279 Problems 280 References 305 Further Reading 306 7 Advanced ExperimentalMethods 309 7.1 Part A: One-Dimensional Techniques 309 7.1.1 T1 Measurements 309 7.1.2 13C Spectral Editing Experiments 311 7.1.2.1 The APT Experiment 311 7.1.2.2 The DEPT Experiment 312 7.1.3 NOE Experiments 313 7.1.3.1 The NOE Difference Experiment 314 7.1.3.2 The Double-Pulse, Field-Gradient, Spin-Echo NOE Experiment 315 7.2 Part B: Two-Dimensional Techniques 316 7.2.1 Two-Dimensional NMR Data-Acquisition Parameters 316 7.2.1.1 Number of Da
• Edition: Second edition
• Publisher Details: Hoboken, New Jersey : John Wiley & Sons, Inc
• Publication Date: 2018
• Extent: 1 online resource
• Subjects: 543.66; Nuclear magnetic resonance spectroscopy
• Languages: English
• ISBNs: 9781119295280
• Related ISBNs: 9781119295273
• Notes: Note: Includes bibliographical references and index.; Note: Description based on CIP data; resource not viewed.
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