It is the aim of the book presented here to give a compass, a kind of
Ariadnes thread, to enable the reader to chart a straightforward path
through the field of NMR experiments for structure determination. It
is a practical course from which the user can learn by doing.
An introductory chapter on the FT NMR spectrometer and on practical
aspects such as probe-head tuning, lock operation, and shimming, is
followed by a series of more than a hundred different experiments,
mostly on 1H and 13C, arranged in chapters according to common
features, each with a short survey at the beginning. The content
ranges from pulse length determinations, routine spectra and test
procedures through decoupling techniques, variable temperature
and LIS measurements, to 1D multipulse sequences and the observation
of heteronuclides such as 6Li, 15N and 17O. More demanding
experiments include those using selective pulses, introducing the
second and third dimensions, and/or using field gradients for
coherence selection.
A standard scheme has been adopted for the detailed description of
the experiments, organized in the following specific sections:
"Purpose" explains the idea and goal of an experiment and refers the
user to related experiments.
"Literature" presents references to the original publication and to
improvements and/or sections in monographs and reviews.
"Pulse Scheme and Phase Cycle" gives the pulse sequence in an
instrument-independent graphic and self-explanatory form, and the
phase cycles of the pulses and the receiver.
"Acquisition" is the main section with instructions on the sample to
be used, the spectrometer configuration, the type of program, and
finally the parameters necessary for the performance of the
experiment. "Processing" describes how to treat the time-domain data.
"Results" presents the spectrum obtained by following the procedure
exactly, as well as some remarks concerning the interpretation.
"Comments" contains an explanation of the most important steps of the
pulse sequence, sometimes with a description using the product
operator formalism for which elementary rules are collected in the
Appendix. "Own Observations" provides space for personal notes.
For those of you interested I include the table of contents:
Chapter 1 The NMR Spectrometer
1.1 Principles of an NMR Spectrometer
1.1.1 The Magnet
1.1.2 The Spectrometer Console
1.1.3 The Work-Station
1.1.4 Maintenance
1.2 Tuning a Probe-Head
1.2.1 Tuning and Matching with a Reflection Meter
1.2.2 Tuning and Matching with an R.F. Bridge and an Oscilloscope
1.2.3 Tuning and Matching with a Wobble Generator
1.3 The Lock Channel
1.4 The Art of Shimming
1.4.1 The Shim Gradients
1.4.2 The Shimming Procedure
Chapter 2 Determination of the Pulse-Length
Exp. 2.1: Determination of the 90 1H Transmitter Pulse-Length
Exp. 2.2: Determination of the 90 13C Transmitter Pulse-Length
Exp. 2.3: Determination of the 90 1H Decoupler Pulse-Length
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: 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: Line-Shape Test for 1H NMR Spectroscopy
Exp. 3.4: Resolution Test for 1H NMR Spectroscopy
Exp. 3.5: Sensitivity Test for 1H NMR Spectroscopy
Exp. 3.6: Line-Shape Test for 13C NMR Spectroscopy
Exp. 3.7: ASTM Sensitivity Test for 13C NMR Spectroscopy
Exp. 3.8: Sensitivity Test for 13C NMR Spectroscopy
Exp. 3.9: Quadrature Image Test
Exp. 3.10: Dynamic Range Test for Signal Amplitudes
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: The Homonuclear SPT Experiment
Exp. 4.6: The Heteronuclear SPT Experiment
Exp. 4.7: 1D Nuclear Overhauser Difference Spectroscopy
Exp. 4.8: 1D NOE Spectroscopy with Multiple Selective
Irradiation
Exp. 4.9: 1H Off-Resonance Decoupled 13C NMR Spectra
Exp. 4.10: The Gated 1H-Decoupling Technique
Exp. 4.11: The Inverse Gated 1H-Decoupling Technique
Exp. 4.12: 1H Single Frequency Decoupling of 13C NMR Spectra
Exp. 4.13: 1H Low-Power Decoupling of 13C NMR Spectra
Exp. 4.14: Measurement of the Heteronuclear Overhauser Effect
Chapter 5 Dynamic NMR Spectroscopy
Exp. 5.1: Low Temperature Calibration with Methanol
Exp. 5.2: High Temperature Calibration with 1,2-Ethanediol
Exp. 5.3: Dynamic 1H NMR Spectroscopy on Dimethylformamide
Exp. 5.4: The Saturation Transfer Experiment
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: Editing 13C NMR Spectra with SEFT
Exp. 6.4: Editing 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: Editing 13C NMR Spectra with DEPT
Exp. 6.10: Editing 13C NMR Spectra with PENDANT
Exp. 6.11: 1D-INADEQUATE
Exp. 6.12: The BIRD Filter
Exp. 6.13: TANGO
Exp. 6.14: The Heteronuclear Double Quantum Filter
Exp. 6.15: Water Suppression by Presaturation
Exp. 6.16: 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 with DANTE
Exp. 7.5: Selective COSY
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 Mechanism
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 PirkleAEs
Reagent
Exp. 8.5: The Relaxation Reagent Cr(acac)3
Exp. 8.6: Quantitative 1H NMR Spectroscopy: Determination of
the Alcohol Content of Polish Vodka
Exp. 8.7: Quantitative 13C NMR Spectroscopy with Inverse Gated
1H-Decoupling
Exp. 8.8: Determination of Paramagnetic Susceptibility by NMR
Exp. 8.9: The CIDNP Effect
Chapter 9 Heteronuclear NMR Spectroscopy
Exp. 9.1: 1H-Decoupled 15N NMR Spectra with DEPT
Exp. 9.2: 1H-Coupled 15N NMR Spectra with DEPT
Exp. 9.3: 19F NMR Spectroscopy
Exp. 9.4: 29Si NMR Spectroscopy with DEPT
Exp. 9.5: 119Sn NMR Spectroscopy
Exp. 9.6: 2H NMR Spectroscopy
Exp. 9.7: 11B NMR Spectroscopy
Exp. 9.8: 17O NMR Spectroscopy with RIDE
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: Double Quantum Filtered COSY with Presaturation
Exp. 10.8: C,H Correlation by Polarization Transfer (HETCOR)
Exp. 10.9: Long-Range C,H Correlation by Polarization Transfer
Exp. 10.10: C,H Correlation via Long-Range Couplings (COLOC)
Exp. 10.11: The Basic HMQC Experiment
Exp. 10.12: Phase-Sensitive HMQC with BIRD Selection and
GARP Decoupling
Exp. 10.13: Phase-Sensitive HMBC with BIRD Selection
Exp. 10.14: The Basic HSQC Experiment
Exp. 10.15: The HOHAHA or TOCSY Experiment
Exp. 10.16: The NOESY Experiment
Exp. 10.17: The CAMELSPIN or ROESY Experiment
Exp. 10.18: The HOESY Experiment
Exp. 10.19: 2D-INADEQUATE
Exp. 10.20: The EXSY Experiment
Chapter 11 NMR Spectroscopy with Pulsed Field Gradients
Exp. 11.1: Calibration of Pulsed Field Gradients
Exp. 11.2: The Pulsed Gradient Spin-Echo Experiment
Exp. 11.3: Gradient-Selected H,H-COSY
Exp. 11.4: Gradient-Selected Phase-Sensitive DQF COSY
Exp. 11.5: Gradient-Selected HMQC
Exp. 11.6: Gradient-Selected HMBC
Exp. 11.7: Phase-Sensitive Gradient-Selected HSQC
Exp. 11.8: Gradient-Selected TOCSY
Exp. 11.9: Gradient-Selected HMQC-TOCSY
Exp. 11.10: Gradient-Selected 1H-Detected 2D INEPT-INADEQUATE
Exp. 11.11: Gradient-Selected SELINCOR
Exp. 11.12: GRECCO
Exp. 11.13: WATERGATE
Chapter 12 The Third Dimension
Exp. 12.1: 3D HMQC-COSY
Exp. 12.2: 3D Gradient-Selected HSQC-TOCSY
Exp. 12.3: 3D H,C,P-Correlation
Appendix 1
Instrument Dialects
Appendix 2
Elementary Product Operator Formalism Rules
Glossary and Index
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Please, excuse the cross posting
stb