High Resolution NMR - 2nd Edition - ISBN: 9780120846610, 9781483293691

High Resolution NMR

2nd Edition

Theory and Chemical Applications

Authors: Author Unknown
eBook ISBN: 9781483293691
Imprint: Academic Press
Published Date: 21st August 1995
Page Count: 354
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Description

High Resolution NMR: Theory and Chemical Applications, Second Edition covers the significant progress in understanding the NMR phenomena, instrumentation, and applications in chemical and biochemistry.

This edition is divided into 14 chapters and begins with the historical developments and theoretical aspects of NMR. Considerable chapters are devoted to the basic principles, chemical shifts, coupling constants, and analysis of complex spectra. Other chapters contain expanded topics on carbon-13, nuclear Overhauser effect, relaxation mechanisms, and the use of superconducting magnets. The remaining chapters examine the concepts of solvent effects, hydrogen bonding, and the use of NMR in quantitative analysis.

This book will prove useful to analytical chemists, biochemists, and researchers.

Table of Contents


Preface to Second Edition

Preface to First Edition

Acknowledgments

1. Introduction

1.1 Historical

1.2 High Resolution NMR

2. The Theory of NMR

2.1 Nuclear Spin and Magnetic Moment

2.2 Classical Mechanical Description of NMR

2.3 Quantum Mechanical Description of NMR

2.4 Effect of the Boltzmann Distribution

2.5 Spin—Lattice Relaxation

2.6 Line Widths

2.7 Saturation

2.8 Macroscopic Magnetization

2.9 The Bloch Equations: Nuclear Induction

2.10 The Rotating Frame of Reference

2.11 Adiabatic Passage; Ringing

Problems

3. Instrumentation and Techniques

3.1 Basic NMR Apparatus

3.2 Requirements for High Resolution NMR

3.3 Modulation and Phase Sensitive Detection

3.4 Field/Frequency Control

3.5 Signal/Noise and Size of Sample

3.6 Fourier Transform Methods

3.7 Intensity Measurements

3.8 References

3.9 Magnetic Susceptibility Measurements

3.10 Frequency Calibration

3.11 Control of Sample Temperature

3.12 Useful Solvents

3.13 Sampling Techniques

3.14 Micro Techniques

Problems

4. Chemical Shifts

4.1 The Origin of Chemical Shifts

4.2 Reference Compounds

4.3 Chemical Shift Scales

4.4 Magnetic Susceptibility Correction

4.5 Empirical Correlations of Chemical Shifts

4.6 Theory of Chemical Shifts

4.7 Effect of Electron Density

4.8 Magnetic Anisotropy and Chemical Shifts

4.9 Ring Currents

4.10 Nuclei Other Than Hydrogen

4.11 Carbon-13

4.12 Tabulations of Chemical Shifts and Spectra

4.13 Empirical Estimation of Chemical Shifts

4.14 Isotope Effects on Chemical Shifts

4.15 Paramagnetic Species

4.16 Lanthanide Shift Reagents

Problems

5. Electron-Coupled Spin—Spin Interactions

5.1 Origin of Spin—Spin Coupling

5.2 Coupling between Groups of Equivalent Nuclei

5.3 First-Order Analysis

5.4 Signs of Coupling Constants

5.5 Theory of Spin—Spin Coupling

5.6 Some Observed Coupling Constants

5.7 Correlation of Coupling Constants with Other Physical Properties

5.8 Tabulations of Coupling Constants

Problems

6. The Use of NMR in Structure Elucidation

6.1 A Systematic Approach to the Interpretation of NMR Spectra

6.2 Some Features of Carbon-13 Spectra

6.3 Structure Elucidation of Polymers

Problems

7. Analysis of Complex Spectra

7.1 Notation

7.2 Energy Levels and Transitions in an AX System

7.3 Quantum Mechanical Formalism

7.4 Nuclear Spin Basis Functions

7.5 The Spin Hamiltonian

7.6 The Two-Spin System without Coupling

7.7 Factoring the Secular Equation

7.8 Two Coupled Spins

7.9 Selection Rules and Intensities

7.10 The AB Spectrum

7.11 Spectral Contributions from Equivalent Nuclei

7.12 Symmetry of Wave Functions

7.13 Summary of Rules for Calculating Spectra

7.14 The Three-Spin System: ABC

7.15 The A2B System

7.16 The A3B System; Subspectral Analysis

7.17 The ABX System

7.18 Analysis of an ABX Spectrum

7.19 Relative Signs of JAX and JBx in an ABX Spectrum

7.20 ABX Patterns; Deceptively Simple Spectra

7.21 “Virtual Coupling”

7.22 The AB'BB' and AA'XX' Systems

7.23 Other Complex Spectra

7.24 Aids in the Analysis of Complex Spectra

7.25 Carbon-13 Satellites

7.26 Effects of Molecular Asymmetry

7.27 Polymer Configuration

7.28 Use of Liquid Crystals as Solvents

Problems

8. Relaxation

8.1 Molecular Motions and Processes for Relaxation in Liquids

8.2 Nuclear Magnetic Dipole Interactions

8.3 Relaxation via Chemical Shift Anisotropy

8.4 Spin—Rotation Relaxation

8.5 Electric Quadrupole Relaxation

8.6 Scalar Relaxation

8.7 Relaxation by Paramagnetic Substances

8.8 Some Chemical Applications

8.9 Measurement of Relaxation Times

Problems

9. Theory and Application of Double Resonance

9.1 Notation and Terminology

9.2 Experimental Techniques

9.3 Theory of Double Resonance

9.4 The Nuclear Overhauser Effect

9.5 Structure Elucidation

9.6 Location of “Hidden” Lines

9.7 Determination of Chemical Shifts

9.8 Relative Signs of Coupling Constants

9.9 Determination of Energy Level Arrangements

9.10 “High Resolution” Spectra in Solids

Problems

10. Pulse Fourier Transform Methods

10.1 RF Pulses and the Free Induction Decay

10.2 Fourier Transformation of the FID

10.3 Instrumental Requirements

10.4 Data Processing in the Computer

10.5 Sensitivity Enhancement by Time Averaging

10.6 Measurement of Relaxation Times

10.7 Two-Dimensional FT-NMR

Problems

11. Exchange Processes: Dynamic NMR

11.1 Spectra of Exchanging Systems

11.2 Theory of Chemical Exchange

11.3 Collapse of Spin Multiplets

11.4 More Complete Theories of Exchange

11.5 Double Resonance and Pulse Techniques

11.6 CIDNP

Problems

12. Solvent Effects and Hydrogen Bonding

12.1 Medium Effects on Chemical Shifts

12.2 Solvent Effects on Coupling Constants

12.3 Solvent Effects on Relaxation and Exchange Rates

12.4 Hydrogen Bonding

Problems

13. Use of NMR in Quantitative Analysis

13.1 Advantages of NMR in Quantitative Analysis

13.2 Drawbacks and Problems in the Use of NMR in Quantitative Analysis

13.3 Some Analytical Uses of NMR

14. Contemporary Developments in NMR

14.1 Solids

14.2 Multinuclear NMR

14.3 Biochemical Studies

14.4 NMR Imaging

References

Appendix A General NMR References

Appendix B Nuclear Spins, Magnetic Moments, and Resonance Frequencies

Appendix C Proton and Carbon-13 NMR Spectra of “Unknowns”

Appendix D Answers to Selected Problems

Index

Details

No. of pages:
354
Language:
English
Copyright:
© Academic Press 1980
Published:
Imprint:
Academic Press
eBook ISBN:
9781483293691

About the Author

Author Unknown