Sample Preparation and Measurements 6.5.1.1 Fluorescence Quantum Yield and Lifetime 138 6.5.1.2 Fluores 6.5.1.3 Solvent Relaxation 144 6.5.1.4 Polarized fluorescence 148 6.5.2 Section Ill Methods 2: Nuclear Magnetic Resonance Spectroscopy 169 Introduction 171 NMR Spectroscopy 177 7.1 Introduction Solution-state H NMR 179 73 Solid-state NMR 187 7.3.1 Dipolar Interaction 188 7.3.2 Chemical Shift Anisotropy 190 7.3.3 Quadrupolar Interaction 191 7.3.4 Magic Angle Spinning(MAS) NMR 194 7.3.5 Ti and Tip Relaxation 192 73. Dynamics 198 7.4 Imaging 199 75 D NMR: The HNCA Pulse Sequence 204 7.6 Conclusion 207 8 Solution NMR Spectroscopy 209 Introduction 209 ID(One-dimensional) NMR Methods 210 8.2.1 Proton Spin Decoupling Experiments 211 8.2.2 Proton Decoupled Difference Spectroscopy 212 8.2.3 Nuclear Overhauser Effect(NOE) Difference Spectroscopy 212 2.4 Selective Population Transfer(SPT) 213 8.2.5 J-Modulated Spin Echo Experiments 213 8.2.5. 1 INEPT(Insensitive Nucleus Enhancement by Polarization Transfer) 214 8.2.5. 2 DEPT(Distortionless Enhancement Polarization Transfer)215 8.2.6 Off-Resonance Decoupling 216 8.2.7 Relaxation Measurements 217 Two-dimensional NMR Experiments 218 J-Resolved NMR Experiments 219 8.3.2 Homonuclear 2D NMR Spectroscopy 223 8.3. 2.1 COSY, Homonuclear Correlated Spectroscopy 223 8.3.2.2 Homonuclear TOCSY, Total Correlated Spectroscopy 226 8.3.2.3 NOESY, Nuclear Overhauser Enhancement Spectroscopy 2286.5.1 Sample Preparation and Measurements 138 6.5.1.1 Fluorescence Quantum Yield and Lifetime 138 6.5.1.2 Fluorescence Quencher 139 6.5.1.3 Solvent Relaxation 144 6.5.1.4 Polarized Fluorescence 148 6.5.2 Special Applications 152 Section III Methods 2: Nuclear Magnetic Resonance Spectroscopy 169 Introduction 171 7 An Introduction to Solution, Solid-State, and Imaging NMR Spectroscopy 177 7.1 Introduction 177 7.2 Solution-state 1 H NMR 179 7.3 Solid-state NMR 187 7.3.1 Dipolar Interaction 188 7.3.2 Chemical Shift Anisotropy 190 7.3.3 Quadrupolar Interaction 191 7.3.4 Magic Angle Spinning (MAS) NMR 194 7.3.5 T1 and T1
Relaxation 195 7.3.6 Dynamics 198 7.4 Imaging 199 7.5 3D NMR: The HNCA Pulse Sequence 204 7.6 Conclusion 207 8 Solution NMR Spectroscopy 209 8.1 Introduction 209 8.2 1D (One-dimensional) NMR Methods 210 8.2.1 Proton Spin Decoupling Experiments 211 8.2.2 Proton Decoupled Difference Spectroscopy 212 8.2.3 Nuclear Overhauser Effect (NOE) Difference Spectroscopy 212 8.2.4 Selective Population Transfer (SPT) 213 8.2.5 J-Modulated Spin Echo Experiments 213 8.2.5.1 INEPT (Insensitive Nucleus Enhancement by Polarization Transfer) 214 8.2.5.2 DEPT (Distortionless Enhancement Polarization Transfer) 215 8.2.6 Off-Resonance Decoupling 216 8.2.7 Relaxation Measurements 217 8.3 Two-dimensional NMR Experiments 218 8.3.1 2D J-Resolved NMR Experiments 219 8.3.2 Homonuclear 2D NMR Spectroscopy 223 8.3.2.1 COSY, Homonuclear Correlated Spectroscopy 223 8.3.2.2 Homonuclear TOCSY, Total Correlated Spectroscopy 226 8.3.2.3 NOESY, Nuclear Overhauser Enhancement Spectroscopy 228 VIII Contents