核磁共振电子书：《150个核磁共振实验 150 Basic-NMR Experiments》

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CONTENTS
INTRODUCTION 8
CHAPTER 2 - DETERMINATION OF THE PULSE-DURATION 9
SUMMARY 9
Experiment 2.1 - Determination of the 90° 1H Transmitter Pulse Duration 9
Experiment 2.2 - Determination of the 90° 13C Transmitter Pulse Duration 10
Experiment 2.3 - Determination of the 90° 1H Decoupler Pulse Duration 10
Experiment 2.4 - The 90° 1H Pulse with Inverse Spectrometer Configuration 11
Experiment 2.5 - The 90° 13C Decoupler Pulse with Inverse Configuration 11
Experiment 2.6 - Composite Pulses 12
Experiment 2.7 - Radiation Damping 13
Experiment 2.8 - Pulse and Receiver Phases 13
Experiment 2.9 - Determination of Radiofrequency Power 14
CHAPTER 3 - ROUTINE NMR SPECTROSCOPY AND STANDARD TESTS 15
SUMMARY 15
Experiment 3.1 - The Standard 1H NMR Experiment 15
Experiment 3.2 - The Standard 13C NMR Experiment 16
Experiment 3.3 - The Application of Window Functions 16
Experiment 3.4 - Computer-aided Spectral Analysis 17
Experiment 3.5 - Line-Shape Test for 1H NMR Spectroscopy 17
Experiment 3.6 - Resolution Test for 1H NMR Spectroscopy 18
Experiment 3.7 - Sensitivity Test for 1H NMR Spectroscopy 18
Experiment 3.8 - Line-Shape Test for 13C NMR Spectroscopy 19
Experiment 3.9 - ASTM Sensitivity Test for 13C NMR Spectroscopy 20
Experiment 3.10 - Sensitivity Test for 13C NMR Spectroscopy 20
Experiment 3.11 - Quadrature Image Test 21
Experiment 3.12 - Dynamic Range Test for Signal Amplitudes 21
Experiment 3.13 – 13° Phase Stability Test 22
CHAPTER 4 - DECOUPLING TECHNIQUES 23
SUMMARY 23
Experiment 4.1 - Decoupler Calibration for Homonuclear Decoupling 23
Experiment 4.2 - Decoupler Calibration for Heteronuclear Decoupling 24
Experiment 4.3 - Low Power Calibration for Heteronuclear Decoupling 25
Experiment 4.4 - Homonuclear Decoupling 25
Experiment 4.5 - Homonuclear Decoupling at Two Frequencies 26
Experiment 4.6 - The Homonuclear SPT Experiment 26
Experiment 4.7 - The Heteronuclear SPT Experiment 27
Experiment 4.8 - 1D Nuclear Overhauser Difference Spectroscopy 27
Experiment 4.9 - 1D NOE Spectroscopy with Multiple Selective Irradiation 28
Experiment 4.10 - 1H Off-Resonance Decoupled 13C NMR Spectra 29
Experiment 4.11 - The Gated 1H-Decoupling Technique 29
Experiment 4.12 - The Inverse Gated 1H-Decoupling Technique 30
Experiment 4.13 - 1H Single Frequency Decoupling of 13C NMR Spectra 30
Experiment 4.14 - 1H Low Power Decoupling of 13C NMR Spectra 31
Experiment 4.15 - Measurement of the Heteronuclear Overhauser Effect 32
CHAPTER 5 - DYNAMIC NMR SPECTROSCOPY 33
SUMMARY 33
Experiment 5.1 - Low Temperature Calibration with Methanol 33
Experiment 5.2 - High Temperature Calibration with 1,2-Ethandiol 33
Experiment 5.3 - Dynamic 1H NMR Spectroscopy on Dimethylformamid 34
Experiment 5.4 - The Saturation Transfer Experiment 34
Experiment 5.5 - Measurement of the Rotating Frame Relaxation Time T1p 35
CHAPTER 6 - 1D MULTIPULSE SEQUENCES 36
SUMMARY 36
Experiment 6.1 - Measurement of the Spin-Lattice Relaxation Time T1 36
Experiment 6.2 - Measurement of the Spin-Spin Relaxation Time T2 37
Experiment 6.3 - 13C NMR Spectra with SEFT 38
Experiment 6.4 - 13C NMR Spectra with APT 38
Experiment 6.5 - The Basic INEPT Technique 39
Experiment 6.6 - INEPT+ 40
Experiment 6.7 - Refocused INEPT 40
Experiment 6.8 - Reverse INEPT 41
Experiment 6.9 - DEPT-135 42
Experiment 6.10 - Editing 13C NMR Spectra with DEPT 42
Experiment 6.11 - Multiplicity Determination with PENDANT 43
Experiment 6.12 - 1D-INADEQUATE 44
Experiment 6.13 - The BIRD Filter 45
Experiment 6.14 - TANGO 45
Experiment 6.15 - The Heteronuclear Double Quantum Filter 46
Experiment 6.16 - Purging with a Spin-Lock Pulse 46
Experiment 6.17 - Water Suppression by Presaturation 47
Experiment 6.18 - Water Suppression by the Jump and Return Method 48
CHAPTER 7 - NMR SPECTROSCOPY WITH SELECTIVE PULSES 49
SUMMARY 49
Experiment 7.1 - Determination of a Shaped 90o 1H Transmitter Pulse 49
Experiment 7.2 - Determination of a Shaped 90o 1H Decoupler Pulse 50
Experiment 7.3 - Determination of a Shaped 90o 13C Decoupler Pulse 50
Experiment 7.4 - Selective Excitation with DANTE 51
Experiment 7.5 - SELCOSY 52
Experiment 7.6 - SELINCOR: Selective Inverse H,C Correlation via 1J (C,H) 52
Experiment 7.7 - SELINQUATE 53
Experiment 7.8 - Selective TOCSY 54
Experiment 7.9 - INAPT 55
Experiment 7.10 - Determination of Long-Range C,H Coupling Constants 56
Experiment 7.11 - SELRESOLV 57
Experiment 7.12 - SERF 57
CHAPTER 8 - AUXILIARY REAGENTS, QUANTITATIVE DETERMINATIONS AND
REACTION MECHANISM 59
SUMMARY 59
Experiment 8.1 - Signal Separation Using a Lanthanide Shift Reagent 59
Experiment 8.2 - Signal Separation of Enantiomers Using a Chiral Shift Reagent 60
Experiment 8.3 - Signal Separation of Enantiomers Using a Chiral Solvating Agent 60
Experiment 8.4 - Determination of Enantiomeric Purity with Pirkle’s Reagent 61
Experiment 8.5 - Determination of Enantiomeric Purity by 31P NMR 61
Experiment 8.6 - Determination of Absolute Configuration by the Advanced Mosher Method 62
Experiment 8.7 - Aromatic Solvent-Induced Shift (ASIS) 62
Experiment 8.8 - NMR Spectroscopy of OH-Protons and H/D Exchange 63
Experiment 8.9 - Isotope Effects on Chemical Shielding 64
Experiment 8.10 - pKa Determination with 13C NMR 64
Experiment 8.11 - The Relaxation Reagent Cr(acac)3 65
Experiment 8.12 - Determination of Paramagnetic Susceptibility by NMR 65
Experiment 8.13 - 1H and 13C NMR of Paramagnetic Compounds 66
Experiment 8.14 - The CIDNP Effect 67
Experiment 8.15 - Quantitative 1H NMR Spectroscopy: Determination of the Alcohol Content of
Polish Vodka 67
Experiment 8.16 - Quantitative 13C NMR Spectroscopy with Inverse Gated 1H-Decoupling 68
Experiment 8.17 - NMR Using Liquid-Crystal Solvents 68
CHAPTER 9 - HETERONUCLEAR NMR SPECROSCOPY 70
SUMMARY 70
Experiment 9.1 - 1H-Decoupled 15N NMR Spectra with DEPT 70
Experiment 9.2 - 1H-Coupled 15N NMR Spectra with DEPT 71
Experiment 9.3 - 19F NMR Spectroscopy 71
Experiment 9.4 - 29Si NMR Spectroscopy with DEPT 72
Experiment 9.5 - 29Si NMR Spectroscopy with Spin-Lock Polarization 73
Experiment 9.6 - 119Sn NMR Spectroscopy 73
Experiment 9.7 - 2H NMR Spectroscopy 74
Experiment 9.8 - 11B NMR Spectroscopy 74
Experiment 9.9 - 17O NMR Spectroscopy with RIDE 75
Experiment 9.10 - 47/49Ti NMR Spectroscopy with ARING 76
CHAPTER 10 - THE SECOND DIMENSION 77
SUMMARY 77
Experiment 10.1 - 2D J-Resolved 1H NMR Spectroscopy 77
Experiment 10.2 - 2D J-Resolved 13C NMR Spectroscopy 78
Experiment 10.3 - The Basic H,H-COSY-Experiment 79
Experiment 10.4 - Long-Range COSY 79
Experiment 10.5 - Phase-Sensitive COSY 80
Experiment 10.6 - Phase-Sensitive COSY-45 81
Experiment 10.7 - E.COSY 82
Experiment 10.8 - Double Quantum Filtered COSY with Presaturation 82
Experiment 10.9 - Fully Coupled C,H Correlation (FUCOUP) 83
Experiment 10.10 - C,H Correlation by Polarization Transfer (HETCOR) 84
Experiment 10.11 - Long-Range C,H Correlation by Polarization Transfer 85
Experiment 10.12 - C,H Correlation via Long-Range Couplings (COLOC) 86
Experiment 10.13 - The Basic HMQC Experiment 86
Experiment 10.14 - Phase-Sensitive HMQC with BIRD Filter and GARP Decoupling 87
Experiment 10.15 - Poor Man’s Gradient HMQC 88
Experiment 10.16 - Phase-Sensitive HMBC with BIRD Filter 89
Experiment 10.17 - The Basic HSQC Experiment 90
Experiment 10.18 - The HOHAHA or TOCSY Experiment 91
Experiment 10.19 - The NOESY Experiment 92
Experiment 10.20 - The CAMELSPIN or ROESY Experiment 93
Experiment 10.21 - The HOESY Experiment 94
Experiment 10.22 - 2D-INADEQUATE 94
Experiment 10.23 - The EXSY Experiment 95
Experiment 10.24 - X, Y Correlation 96
CHAPTER 11 - NMR SPECTROSCOPY WITH PULSED FIELD GRADIENTS 98
SUMMARY 98
Experiment 11.1 - Calibration of Pulsed Field Gradients 98
Experiment 11.2 - Gradient Preemphasis 99
Experiment 11.3 - Gradient Amplifier Test 99
Experiment 11.4 - Determination of Pulsed Field Gradient Ring-Down Delays 100
Experiment 11.5 - The Pulsed Gradient Spin-Echo Experiment 100
Experiment 11.6 - Excitation Pattern of Selective Pulses 101
Experiment 11.7 - The Gradient zz-Filter 102
Experiment 11.8 - gs-SELCOSY 102
Experiment 11.9 - gs-SELTOCSY 103
Experiment 11.10 - DPFGSE-NOE 104
Experiment 11.11 - gs-SELINCOR 105
Experiment 11.12 - GRECCO 106
Experiment 11.13 - WATERGATE 106
Experiment 11.14 - Water Suppression by Excitation Sculpting 107
CHAPTER 12 - 2D NMR SPECTROSCOPY WITH FIELD GRADIENTS 108
SUMMARY 108
Experiment 12.1 - gs-COSY 108
Experiment 12.2 - Phase-Sensitive gs-DQF-COSY 109
Experiment 12.3 - gs-HMQC 110
Experiment 12.4 - gs-HMBC 110
Experiment 12.5 - ACCORD-HMBC 111
Experiment 12.6 - Phase-Sensitive gs-HSQC with Sensitivity Enhancement 112
Experiment 12.7 - gs-TOCSY 113
Experiment 12.8 - gs-HMQC-TOCSY 114
Experiment 12.9 - 2Q-HMBC 115
Experiment 12.10 - Gradient-Selected 1H-Detected 2D INEPT-INADEQUATE 116
Experiment 12.11 - gs-NOESY 117
Experiment 12.12 - gs-HSQC-NOESY 118
Experiment 12.13 - gs-HOESY 119
Experiment 12.14 - 1H, 15N Correlation with gs-HMQC 119
CHAPTER 13 - THE THIRD DIMENSION 121
SUMMARY 121
Experiment 13.1 - 3D HMQC-COSY 121
Experiment 13.2 - 3D gs-HSQC-TOCSY 122
Experiment 13.3 - 3D H,C,P-Correlation 122
Experiment 13.4 - 3D HMBC 123
CHAPTER 14 - SOLID-STATE NMR SPECTROSCOPY 124
SUMMARY 124
Experiment 14.1 - Shimming Solid-State Probe-Heads 124
Experiment 14.2 – Adjusting the Magic Angle 125
Experiment 14.3 - Hartmann-Hahn Matching 126
Experiment 14.4 – The Basic CP/MAS Experiment 127
Experiment 14.5 - TOSS 127
Experiment 14.6 - SELTICS 128
Experiment 14.7 - Multiplicity Determination in the Solid-State 129