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Contents
Preface
Chapter 1 The NMR Spectrometer
1.1 Components of an NMR Spectrometer
1.1.1 The Magnet
1.1.2 The Spectrometer Cabinet
1.1.3 The Computer
1.1.4 Maintenance
1.2 Tuning a Probe-Head
1.3 The Lock Channel
1.4 The Art of Shimming
1.4.1 The Shim Gradients
1.4.2 The Shimming Procedure
1.4.3 Gradient Shimming
Chapter 2 Determination of Pulse-Duration
Exp. 2.1: Determination of the 90° 1H Transmitter Pulse-Duration
Exp. 2.2: Determination of the 90° 13C Transmitter Pulse-Duration
Exp. 2.3: Determination of the 90° 1H Decoupler Pulse-Duration
Exp. 2.4: The 90° 1H Pulse with Inverse Spectrometer Configuration
Exp. 2.5: The 90° 13C Decoupler Pulse with Inverse Configuration
Exp. 2.6: Composite Pulses
Exp. 2.7: Radiation Damping
Exp. 2.8: P ulse and Receiver Phases
Exp. 2.9: Determination of Radiofrequency Power
Chapter 3 Routine NMR Spectroscopy and Standard Tests
Exp. 3.1: The Standard 1H NMR Experiment
Exp. 3.2: The Standard 13C NMR Experiment
Exp. 3.3: The Application of Window Functions
Exp. 3.4: Computer-Aided Spectral Analysis
Exp. 3.5: Line Shape Test for 1H NMR Spectroscopy
Exp. 3.6: Resolution Test for 1H NMR Spectroscopy
Exp. 3.7: Sensitivity Test for 1H NMR Spectroscopy
Exp. 3.8: Line Shape Test for 13C NMR Spectroscopy
Exp. 3.9: ASTM Sensitivity Test for 13C NMR Spectroscopy
Exp. 3.10 :Sensitivity Test for 13C NMR Spectroscopy
Exp. 3.11: Quadrature Image Test
Exp. 3.12: Dynamic Range Test for Signal Amplitudes
Exp. 3.13: 13° Phase Stability Test
Exp. 3.14: Radiofrequency Field Homogeneity
Chapter 4 Decoupling Techniques
Exp. 4.1: Decoupler Calibration for Homonuclear Decoupling
Exp. 4.2: Decoupler Calibration for Heteronuclear Decoupling
Exp. 4.3: Low-Power Calibration for Heteronuclear Decoupling
Exp. 4.4: Homonuclear Decoupling
Exp. 4.5: Homonuclear Decoupling at Two Frequencies
Exp. 4.6: The Homonuclear SPT Experiment
Exp. 4.7: The Heteronuclear SPT Experiment
Exp. 4.8: The Basic Homonuclear NOE Difference Experiment
Exp. 4.9: 1D Nuclear Overhauser Difference Spectroscopy
Exp. 4.10: 1D NOE Spectroscopy with Multiple Selective Irradiation
Exp. 4.11: 1H Off-Resonance Decoupled 13C NMR Spectra
Exp. 4.12: The Gated 1H-Decoupling Technique
Exp. 4.13: The Inverse Gated 1H-Decoupling Technique
Exp. 4.14: 1H Single-Frequency Decoupling of 13C NMR Spectra
Exp. 4.15: 1H Low-Power Decoupling of 13C NMR Spectra
Exp. 4.16: Measurement of the Heteronuclear Overhauser Effect
Chapter 5 Dynamic NMR Spectroscopy
Exp. 5.1: Low-Temperature Calibration Using Methanol
Exp. 5.2: High-Temperature Calibration Using 1,2-Ethanediol
Exp. 5.3: Dynamic 1H NMR Spectroscopy on Dimethylformamide
Exp. 5.4: The Saturation Transfer Experiment
Exp. 5.5: Measurement of the Rotating-Frame Relaxation Time T1
Chapter 6 1D Multipulse Sequences
Exp. 6.1: Measurement of the Spin Lattice Relaxation Time T1
Exp. 6.2: Measurement of the Spin Spin Relaxation Time T2
Exp. 6.3: 13C NMR Spectra with SEFT
Exp. 6.4: 13C NMR Spectra with APT
Exp. 6.5: The Basic INEPT Technique
Exp. 6.6: INEPT+
Exp. 6.7: Refocused INEPT
Exp. 6.8: Reverse INEPT
Exp. 6.9: DEPT-135
Exp. 6.10: Editing 13C NMR Spectra Using DEPT
Exp. 6.11: DEPTQ
Exp. 6.12: Multiplicity Determination Using PENDANT
Exp. 6.13: 1D-INADEQUATE
Exp. 6.14: The BIRD Filter
Exp. 6.15: TANGO
Exp. 6.16: The Heteronuclear Double-Quantum Filter
Exp. 6.17: Purging with a Spin-Lock Pulse
Exp. 6.18: Water Suppression by Presaturation
Exp. 6.19: Water Suppression by the Jump-and-Return Method
Chapter 7 NMR Spectroscopy with Selective Pulses
Exp. 7.1: Determination of a Shaped 90° 1H Transmitter Pulse
Exp. 7.2: Determination of a Shaped 90° 1H Decoupler Pulse
Exp. 7.3: Determination of a Shaped 90° 13C Decoupler Pulse
Exp. 7.4: Selective Excitation Using DANTE
Exp. 7.5: SELCOSY
Exp. 7.6: SELINCOR: Selective Inverse H,C Correlation via 1J(C,H)
Exp. 7.7: SELINQUATE
Exp. 7.8: Selective TOCSY
Exp. 7.9: INAPT
Exp. 7.10: Determination of Long-Range C,H Coupling Constants
Exp. 7.11: SELRESOLV
Exp. 7.12: SERF
Chapter 8 Auxiliary Reagents, Quantitative Determinations, and Reaction Mechanisms
Exp. 8.1: Signal Separation Using a Lanthanide Shift Reagent
Exp. 8.2: Signal Separation of Enantiomers Using a Chiral Shift Reagent
Exp. 8.3: Signal Separation of Enantiomers Using a Chiral Solvating Agent
Exp. 8.4: Determination of Enantiomeric Purity with Pirkle's Reagent
Exp. 8.5: Determination of Enantiomeric Purity by 31P NMR
Exp. 8.6: Determination of Absolute Configuration by the Advanced Mosher Method
Exp. 8.7: Aromatic Solvent-Induced Shift (ASIS)
Exp. 8.8: NMR Spectroscopy of OH Protons and H/D Exchange
Exp. 8.9: Water Suppression Using an Exchange Reagent
Exp. 8.10: Isotope Effects on Chemical Shielding
Exp. 8.11: pKa Determination by 13C NMR
Exp. 8.12: Determination of Association Constants Ka
Exp. 8.13: Saturation Transfer Difference NMR
Exp. 8.14: The Relaxation Reagent Cr(acac)3
Exp. 8.15: Determination of Paramagnetic Susceptibility by NMR
Exp. 8.16: 1H and 13C NMR of Paramagnetic Compounds
Exp. 8.17: The CIDNP Effect
Exp. 8.18: Quantitative 1H NMR Spectroscopy: Determination of the Alcohol Content of Polish Vodka
Exp. 8.19: Quantitative 13C NMR Spectroscopy with Inverse Gated 1H-Decoupling
Exp. 8.20: NMR Using Liquid-Crystal Solvents
Chapter 9 Heteronuclear NMR Spectroscopy
Exp. 9.1: 1H-Decoupled 15N NMR Spectra Using DEPT
Exp. 9.2: 1H-Coupled 15N NMR Spectra Using DEPT
Exp. 9.3: 19F NMR Spectroscopy
Exp. 9.4: 29Si NMR Spectroscopy Using DEPT
Exp. 9.5: 29Si NMR Spectroscopy Using Spin-Lock Polarization
Exp. 9.6: 119Sn NMR Spectroscopy
Exp. 9.7: 2H NMR Spectroscopy
Exp. 9.8: 11B NMR Spectroscopy
Exp. 9.9: 17O NMR Spectroscopy Using RIDE
Exp. 9.10: 47/49Ti NMR Spectroscopy Using ARING
Chapter 10 The Second Dimension
Exp. 10.1: 2D J-Resolved 1H NMR Spectroscopy
Exp. 10.2: 2D J-Resolved 13C NMR Spectroscopy
Exp. 10.3: The Basic H,H-COSY Experiment
Exp. 10.4: Long-Range COSY
Exp. 10.5: Phase-Sensitive COSY
Exp. 10.6: Phase-Sensitive COSY-45
Exp. 10.7: E.COSY
Exp. 10.8: Double-Quantum-Filtered COSY with Presaturation
Exp. 10.9: Fully Coupled C,H Correlation (FUCOUP)
Exp. 10.10: C,H-Correlation by Polarization Transfer (HETCOR)
Exp. 10.11: Long-Range C,H-Correlation by Polarization Transfer
Exp. 10.12: C,H Correlation via Long-Range Couplings (COLOC)
Exp. 10.13: The Basic HMQC Experiment
Exp. 10.14: Phase-Sensitive HMQC with BIRD Filter and GARP Decoupling
Exp. 10.15: Poor Man's Gradient HMQC
Exp. 10.16: Phase-Sensitive HMBC with BIRD Filter
Exp. 10.17: The Basic HSQC Experiment
Exp. 10.18: The HOHAHA or TOCSY Experiment
Exp. 10.19: HETLOC
Exp. 10.20: The NOESY Experiment
Exp. 10.21: The CAMELSPIN or ROESY Experiment
Exp. 10.22: The HOESY Experiment
Exp. 10.23: 2D-INADEQUATE
Exp. 10.24: The EXSY Experiment
Exp. 10.25: X,Y-Correlation
Chapter 11 1D NMR Spectroscopy with Pulsed Field Gradients
Exp. 11.1: Calibration of Pulsed Field Gradients
Exp. 11.2: Gradient Pre-emphasis
Exp. 11.3: Gradient Amplifier Test
Exp. 11.4: Determination of Pulsed Field Gradient Ring-Down Delays
Exp. 11.5: The Pulsed Field Gradient Spin-Echo Experiment
Exp. 11.6: Excitation Pattern of Selective Pulses
Exp. 11.7: The Gradient Heteronuclear Double-Quantum Filter
Exp. 11.8: The Gradient zz-Filter
Exp. 11.9: The Gradient-Selected Dual Step Low-Pass Filter
Exp. 11.10: gs-SELCOSY
Exp. 11.11: gs-SELTOCSY
Exp. 11.12: DPFGSE-NOE
Exp. 11.13: gs-SELINCOR
Exp. 11.14: SELINCOR-TOCSY
Exp. 11.15: GRECCO
Exp. 11.16: WATERGATE
Exp. 11.17: Water Suppression by Excitation Sculpting
Exp. 11.18: Solvent Suppression Using WET
Exp. 11.19: DOSY
Exp. 11.20: INEPT-DOSY
Exp. 11.21: DOSY-HMQC
Chapter 12 2D NMR Spectroscopy With Field Gradients
Exp. 12.1: gs-COSY
Exp. 12.2: Constant-Time COSY
Exp. 12.3: Phase-Sensitive gs-DQF-COSY
Exp. 12.4: gs-HMQC
Exp. 12.5: gs-HMBC
Exp. 12.6: ACCORD-HMBC
Exp. 12.7: HMSC
Exp. 12.8: Phase-Sensititive gs-HSQC with Sensitivity Enhancement
Exp. 12.9: Edited HSQC with Sensitivity Enhancement
Exp. 12.10: HSQC with Adiabatic Pulses for High-Field Instruments
Exp. 12.11: gs-TOCSY
Exp. 12.12: gs-HMQC-TOCSY
Exp. 12.13: gs-HETLOC
Exp. 12.14: gs-J-Resolved HMBC
Exp. 12.15: 2Q-HMBC
Exp. 12.16: 1H-Detected 2D INEPT-INADEQUATE
Exp. 12.17: 1,1-ADEQUATE
Exp. 12.18: 1,n-ADEQUATE
Exp. 12.19: gs-NOESY
Exp. 12.20: gs-HSQC-NOESY
Exp. 12.21: gs-HOESY
Exp. 12.22: 1H,15N Correlation with gs-HMQC
Chapter 13 The Third Dimension
Exp. 13.1: 3D HMQC-COSY
Exp. 13.2: 3D gs-HSQC-TOCSY
Exp. 13.3: 3D H,C,P-Correlation
Exp. 13.4: 3D HMBC
Chapter 14 Solid-State NMR Spectroscopy
Exp. 14.1: Shimming Solid-State Probe-Heads
Exp. 14.2: Adjusting the Magic Angle
Exp. 14.3: Hartmann Hahn Matching
Exp. 14.4: The Basic CP/MAS Experiment
Exp. 14.5: TOSS
Exp. 14.6: SELTICS
Exp. 14.7: Connectivity Determination in the Solid State
Exp. 14.8: REDOR
Exp. 14.9: High-Resolution Magic-Angle Spinning
Chapter 15 Protein NMR
Exp. 15.1: Pulse Determination for Protein NMR
Exp. 15.2: HN-HSQC
Exp. 15.3: HC-HSQC
Exp. 15.4: MUSIC
Exp. 15.5: HN-Correlation using TROSY
Exp. 15.6: HN-TOCSY-HSQC
Exp. 15.7: HNCA
Exp. 15.8: HN(CO)CA
Exp. 15.9: HNCO
Exp. 15.10: HN(CA)CO
Exp. 15.11: HCACO
Exp. 15.12: HCCH-TOCSY
Exp. 15.13: CBCANH
Exp. 15.14: CBCA(CO)NH
Exp. 15.15: HBHA(CBCACO)NH
Exp. 15.16: HN(CA)NNH
Exp. 15.17: HN-NOESY-HSQC
Exp. 15.18: HC-NOESY-HSQC
Exp. 15.19: 3D HCN-NOESY
Exp. 15.20: HNCA-J
Appendix 1
Pulse Programs
Appendix 2
Instrument Dialects
Appendix 3
Classification of Experiments
Appendix 4
Elementary Product Operator Formalism Rules
Appendix 5
Chemical Shift and Spin-Coupling Data for Ethyl Crotonate and Strychnine
Glossary and Index
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