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Introduction to Solid-State NMR Spectroscopy de Melinda J. Duer

Introduction to Solid-State NMR Spectroscopy

Autor Melinda J. Duer, Duer
en Limba Engleză Paperback – 16 iul 2005
Introduction to Solid State NMR Spectroscopy is written for undergraduate and graduate students of chemistry, either taking a course in advanced or solid-state nuclear magnetic resonance spectroscopy or undertaking research projects where solid-state NMR is likely to be a major investigative technique. It will also serve as a practical introduction in industry, where the techniques can provide new or complementary information to supplement other investigative techniques.


By covering solid-state NMR spectroscopy in a clear, straightforward and approachable way with detailed descriptions of the major solid-state NMR experiments focussing on what the experiments do and what they tell the researcher, this book will serve as an ideal introduction to the subject. These descriptions are backed up by separate mathematical explanations for those who wish to gain a more sophisticated quantitative understanding of the phenomena. With additional coverage of the practical implementation of solid-state NMR experiments integrated into the discussion, this book will be essential reading for all those using, or about to use, solid-state NMR spectroscopy.



Dr Melinda Duer is a senior lecturer in the Department of Chemistry at the University of Cambridge, Cambridge, UK.

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Specificații

ISBN-13: 9781405109147
ISBN-10: 1405109149
Pagini: 368
Ilustrații: 134
Dimensiuni: 178 x 254 x 20 mm
Greutate: 0.69 kg
Editura: Wiley
Locul publicării:Chichester, United Kingdom

Public țintă

Postgraduate and advanced undergraduate students in chemistry. Industrial researchers encountering solid state NMR spectroscopy for the first time.

Notă biografică

Dr Melinda Duer is a senior lecturer in the Department of Chemistry at the University of Cambridge, Cambridge, UK

Cuprins

Preface, xii

Acknowledgements, xv

1 The Basics of NMR, 1

1.1 The vector model of pulsed NMR, 1

1.1.1 Nuclei in a static, uniform magnetic field, 2

1.1.2 The effect of rf pulses, 3

1.2 The quantum mechanical picture: hamiltonians and the Schrödinger equation, 5

Box 1.1 Quantum mechanics and NMR, 6

Wavefunctions, 6

Operators, physical observables and expectation values, 7

Schrödinger's equation, eigenfunctions and eigenvalues, 7

Spin operators and spin states, 8

Dirac's bra-ket notation, 11

Matrices, 11

1.2.1 Nuclei in a static, uniform field, 12

1.2.2 The effect of rf pulses, 15

Box 1.2 Exponential operators, rotation operators and rotations, 19

Rotation of vectors, wavefunctions and operators (active rotations), 20

Rotation of axis frames, 23

Representation of rf fields, 25

Euler angles, 25

Rotations with Euler angles, 26

Rotation of Cartesian axis frames, 27

1.3 The density matrix representation and coherences, 29

1.3.1 Coherences and populations, 30

1.3.2 The density operator at thermal equilibrium, 33

1.3.3 Time evolution of the density matrix, 34

1.4 Nuclear spin interactions, 37

1.4.1 Interaction tensors, 41

1.5 General features of Fourier transform NMR experiments, 43

1.5.1 Multidimensional NMR, 43

1.5.2 Phase cycling, 46

1.5.3 Quadrature detection, 48

Box 1.3 The NMR spectrometer, 53

Generating rf pulses, 53

Detecting the NMR signal, 56

Notes, 58

References, 59

2 Essential Techniques for Solid-State NMR, 60

2.1 Introduction, 60

2.2 Magic-angle spinning (MAS), 61

2.2.1 Spinning sidebands, 62

2.2.2 Rotor or rotational echoes, 67

2.2.3 Removing spinning sidebands, 67

2.2.4 Setting the magic-angle and spinning rate, 72

2.2.5 Magic-angle spinning for homonuclear dipolar couplings, 75

2.3 Heteronuclear decoupling, 77

2.3.1 High-power decoupling, 78

2.3.2 Other heteronuclear decoupling sequences, 81

2.4 Homonuclear decoupling, 83

2.4.1 Implementing homonuclear decoupling sequences, 83

Box 2.1 Average hamiltonian theory and the toggling frame, 86

Average hamiltonian theory, 86

The toggling frame and the WAHUHA pulse sequence, 89

2.5 Cross-polarization, 96

2.5.1 Theory, 97

2.5.2 Setting up the cross-polarization experiment, 101

Box 2.2 Cross-polarization and magic-angle spinning, 106

2.6 Echo pulse sequences, 110

Notes, 113

References, 114

3 Shielding and Chemical Shift: Theory and Uses, 116

3.1 Theory, 116

3.1.1 Introduction, 116

3.1.2 The chemical shielding hamiltonian, 117

3.1.3 Experimental manifestations of the shielding tensor, 120

3.1.4 Definition of the chemical shift, 123

3.2 The relationship between the shielding tensor and electronic structure, 125

3.3 Measuring chemical shift anisotropies, 131

3.3.1 Magic-angle spinning with recoupling pulse sequences, 132

3.3.2 Variable-angle spinning experiments, 135

3.3.3 Magic-angle turning, 138

3.3.4 Two-dimensional separation of spinning sideband patterns, 141

3.4 Measuring the orientation of chemical shielding tensors in the molecular frame for structure determination, 145

Notes, 149

References, 149

4 Dipolar Coupling: Theory and Uses, 151

4.1 Theory, 151

4.1.1 Homonuclear dipolar coupling, 154

Box 4.1 Basis sets for multispin systems, 156

4.1.2 The effect of homonuclear dipolar coupling on a spin system, 157

4.1.3 Heteronuclear dipolar coupling, 160

4.1.4 The effect of heteronuclear dipolar coupling on the spin system, 162

4.1.5 Heteronuclear spin dipolar coupled to a homonuclear network of spins, 163

4.1.6 The spherical tensor form of the dipolar hamiltonian, 164

Box 4.2 The dipolar hamiltonian in terms of spherical tensor operators, 164

Spherical tensor operators, 165

Interaction tensors, 167

The homonuclear dipolar hamiltonian under static and MAS conditions, 167

4.2 Introduction to the uses of dipolar coupling, 172

4.3 Techniques for measuring homonuclear dipolar couplings, 175

4.3.1 Recoupling pulse sequences, 175

Box 4.3 Analysis of the DRAMA pulse sequence, 180

Simulating powder patterns from the DRAMA experiment, 184

4.3.2 Double-quantum filtered experiments, 185

Box 4.4 Excitation of double-quantum coherence under magic-angle spinning, 189

The form of the reconversion pulse sequence: the need for timereversal symmetry, 191

Analysis of the double-quantum filtered data, 195

Box 4.5 Analysis of the C7 pulse sequence for exciting double-quantum coherence in dipolar-coupled spin pairs, 196

4.3.3 Rotational resonance, 199

Box 4.6 Theory of rotational resonance, 202

Effect of H ¿ ¿ term on the density operator, 203

The hamiltonian in the new rotated frame, 204

The average hamiltonian, 205

4.4 Techniques for measuring heteronuclear dipolar couplings, 207

4.4.1 Spin-echo double resonance (SEDOR), 207

4.4.2 Rotational-echo double resonance (REDOR), 208

Box 4.7 Analysis of the REDOR experiment, 210

4.5 Techniques for dipolar-coupled quadrupolar-spin-1-2 pairs, 215

4.5.1 Transfer of population in double resonance (TRAPDOR), 216

4.5.2 Rotational-echo adiabatic-passage double-resonance (REAPDOR), 219

4.6 Techniques for measuring dipolar couplings between quadrupolar nuclei, 220

4.7 Correlation experiments, 221

4.7.1 Homonuclear correlation experiments for spin-1-2 systems, 221

4.7.2 Homonuclear correlation experiments for quadrupolar spin systems, 224

4.7.3 Heteronuclear correlation experiments for spin-1-2, 226

4.8 Spin-counting experiments, 227

4.8.1 The formation of multiple-quantum coherences, 228

4.8.2 Implementation of spin-counting experiments, 231

Notes, 232

References, 233

5 Quadrupole Coupling: Theory and Uses, 235

5.1 Introduction, 235

5.2 Theory, 237

5.2.1 The quadrupole hamiltonian, 237

Box 5.1 The quadrupole hamiltonian in terms of spherical tensor operators: the effect of the rotating frame and magic-angle spinning, 242

The quadrupole hamiltonian in terms of spherical tensor operators, 242

The effect of the rotating frame: first- and second-order average hamiltonians for the quadrupole interaction, 243

The energy levels under quadrupole coupling, 248

The effect of magic-angle spinning, 248

5.2.2 The effect of rf pulses, 249

5.2.3 The effects of quadrupolar nuclei on the spectra of spin-1-2 nuclei, 252

5.3 High-resolution NMR experiments for half-integer quadrupolar nuclei, 255

5.3.1 Magic-angle spinning (MAS), 256

5.3.2 Double rotation (DOR), 259

5.3.3 Dynamic-angle spinning (DAS), 260

5.3.4 Multiple-quantum magic-angle spinning (MQMAS), 263

5.3.5 Satellite transition magic-angle spinning (STMAS), 268

5.3.6 Recording two-dimensional datasets for DAS, MQMAS and STMAS, 275

5.4 Other techniques for half-integer quadrupole nuclei, 280

5.4.1 Quadrupole nutation, 282

5.4.2 Cross-polarization, 285

Notes, 290

References, 291

6 NMR Techniques for Studying Molecular Motion in Solids, 293

6.1 Introduction, 293

6.2 Powder lineshape analysis, 296

6.2.1 Simulating powder pattern lineshapes, 297

6.2.2 Resolving powder patterns, 305

6.2.3 Using homonuclear dipolar-coupling lineshapes - the WISE experiment, 311

6.3 Relaxation time studies, 313

6.4 Exchange experiments, 316

6.4.1 Achieving pure absorption lineshapes in exchange spectra, 318

6.4.2 Interpreting two-dimensional exchange spectra, 320

6.5 2H NMR, 322

6.5.1 Measuring 2H NMR spectra, 323

6.5.2 2H lineshape simulations, 328

6.5.3 Relaxation time studies, 329

6.5.4 2H exchange experiments, 330

6.5.5 Resolving 2H powder patterns, 332

Notes, 334

References, 335

Appendix A NMR Properties of Commonly Observed Nuclei, 336

Appendix B The General Form of a Spin Interaction Hamiltonian in Terms of Spherical Tensors and Spherical Tensor Operators, 337

References, 343

Index, 344

Descriere

Covers solid-state NMR spectroscopy and offers descriptions of the major experiments focussing on what the experiments do and what they tell the researcher. This book offers an introduction to the subject. It features descriptions backed up by separate mathematical explanations. It is intended for those using solid-state NMR spectroscopy.