Magnetic resonance Books

Book SynopsisThis text discusses the high-resolution NMR of liquid samples and concentrates exclusively on spin-half nuclei (mainly 1 H and 13 C). It is aimed at people who are familiar with the use of routine NMR for structure determination and who wish to deepen their understanding of just exactly how NMR experiments work.Table of ContentsPreface v Preface to the first edition vi 1 What this book is about and who should read it 1 1.1 How this book is organized 2 1.2 Scope and limitations 3 1.3 Context and further reading 3 1.4 On-line resources 4 1.5 Abbreviations and acronyms 4 2 Setting the scene 5 2.1 NMR frequencies and chemical shifts 5 2.2 Linewidths, lineshapes and integrals 9 2.3 Scalar coupling 10 2.4 The basic NMR experiment 13 2.5 Frequency, oscillations and rotations 15 2.6 Photons 20 2.7 Moving on 21 2.8 Further reading 21 2.9 Exercises 22 3 Energy levels and NMR spectra 23 3.1 The problem with the energy level approach 24 3.2 Introducing quantum mechanics 26 3.3 The spectrum from one spin 31 3.4 Writing the Hamiltonian in frequency units 34 3.5 The energy levels for two coupled spins 35 3.6 The spectrum from two coupled spins 38 3.7 Three spins 40 3.8 Summary 44 3.9 Further reading 44 3.10 Exercises 45 4 The vector model 47 4.1 The bulk magnetization 47 4.2 Larmor precession 50 4.3 Detection 51 4.4 Pulses 52 4.5 On-resonance pulses 57 4.6 Detection in the rotating frame 60 4.7 The basic pulse–acquire experiment 60 4.8 Pulse calibration 61 4.9 The spin echo 63 4.10 Pulses of different phases 66 4.11 Off-resonance effects and soft pulses 67 4.12 Moving on 71 4.13 Further reading 71 4.14 Exercises 72 5 Fourier transformation and data processing 77 5.1 How the Fourier transform works 78 5.2 Representing the FID 82 5.3 Lineshapes and phase 83 5.4 Manipulating the FID and the spectrum 90 5.5 Zero filling 99 5.6 Truncation 100 5.7 Further reading 101 5.8 Exercises 102 6 The quantum mechanics of one spin 105 6.1 Introduction 105 6.2 Superposition states 106 6.3 Some quantum mechanical tools 107 6.4 Computing the bulk magnetization 112 6.5 Summary 117 6.6 Time evolution 118 6.7 RF pulses 123 6.8 Making faster progress: the density operator 126 6.9 Coherence 134 6.10 Further reading 135 6.11 Exercises 136 7 Product operators 139 7.1 Operators for one spin 139 7.2 Analysis of pulse sequences for a one-spin system 143 7.3 Speeding things up 146 7.4 Operators for two spins 149 7.5 In-phase and anti-phase terms 152 7.6 Hamiltonians for two spins 157 7.7 Notation for heteronuclear spin systems 157 7.8 Spin echoes and J-modulation 158 7.9 Coherence transfer 166 7.10 The INEPT experiment 167 7.11 Selective COSY 171 7.12 Coherence order and multiple-quantum coherences 173 7.13 Summary 178 7.14 Further reading 179 7.15 Exercises 180 8 Two-dimensional NMR 183 8.1 The general scheme for two-dimensional NMR 184 8.2 Modulation and lineshapes 187 8.3 COSY 190 8.4 DQF COSY 200 8.5 Double-quantum spectroscopy 203 8.6 Heteronuclear correlation spectra 208 8.7 HSQC 209 8.8 HMQC 212 8.9 Long-range correlation: HMBC 215 8.10 HETCOR 220 8.11 TOCSY 221 8.12 Frequency discrimination and lineshapes 226 8.13 Further reading 236 8.14 Exercises 238 9 Relaxation and the NOE 241 9.1 The origin of relaxation 242 9.2 Relaxation mechanisms 249 9.3 Describing random motion – the correlation time 251 9.4 Populations 258 9.5 Longitudinal relaxation behaviour of isolated spins 263 9.6 Longitudinal dipolar relaxation of two spins 267 9.7 The NOE 274 9.8 Transverse relaxation 286 9.9 Homogeneous and inhomogeneous broadening 300 9.10 Relaxation due to chemical shift anisotropy 304 9.11 Cross correlation 306 9.12 Summary 311 9.13 Further reading 311 9.14 Exercises 313 10 Advanced topics in two-dimensional NMR 319 10.1 Product operators for three spins 320 10.2 COSY for three spins 325 10.3 Reduced multiplets in COSY spectra 330 10.4 Polarization operators 337 10.5 ZCOSY 345 10.6 HMBC 347 10.7 Sensitivity-enhanced experiments 349 10.8 Constant time experiments 353 10.9 TROSY 358 10.10 Double-quantum spectroscopy of a three-spin system 366 10.11 Further reading 374 10.12 Exercises 376 11 Coherence selection: phase cycling and field gradient pulses 381 11.1 Coherence order 382 11.2 Coherence transfer pathways 387 11.3 Frequency discrimination and lineshapes 389 11.4 The receiver phase 391 11.5 Introducing phase cycling 395 11.6 Some phase cycling ‘tricks’ 401 11.7 Axial peak suppression 403 11.8 CYCLOPS 403 11.9 Examples of practical phase cycles 404 11.10 Concluding remarks about phase cycling 408 11.11 Introducing field gradient pulses 409 11.12 Features of selection using gradients 416 11.13 Examples of using gradient pulses 421 11.14 Advantages and disadvantages of coherence selection with gradients 426 11.15 Suppression of zero-quantum coherence 426 11.16 Selective excitation with the aid of gradients 432 11.17 Further reading 435 11.18 Exercises 436 12 Equivalent spins and spin system analysis 441 12.1 Strong coupling in a two-spin system 442 12.2 Chemical and magnetic equivalence 446 12.3 Product operators for AXn (InS) spin systems 450 12.4 Spin echoes in InS spin systems 455 12.5 INEPT in InS spin systems 458 12.6 DEPT 462 12.7 Spin system analysis 468 12.8 Further reading 477 12.9 Exercises 478 13 How the spectrometer works 483 13.1 The magnet 483 13.2 The probe 485 13.3 The transmitter 486 13.4 The receiver 488 13.5 Digitizing the signal 489 13.6 Quadrature detection 491 13.7 The pulse programmer 493 13.8 Further reading 493 13.9 Exercises 494 A Some mathematical topics 495 A.1 The exponential function and logarithms 495 A.2 Complex numbers 497 A.3 Trigonometric identities 499 A.4 Further reading 500 Index 501

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Book SynopsisCharacterisation Methods in Inorganic Chemistry provides a fresh alternative to the existing theoretical and descriptive inorganic chemistry texts by adopting a techniques-based approach and providing problem-solving opportunities to show how analytical methods are used to help us characterise inorganic compounds. The text covers the full range of analytical techniques employed by inorganic chemists, emphasizing those in most frequent use: NMR, diffraction, UV-Vis spectroscopy, and IR. The additional coverage on other techniques allows readers to study these less widely used methods when relevant to their specific course material. Each chapter follows a clear, structured format, which begins with a brief introduction to the technique and basic theory behind it before moving on to data collection and analysis, typical data and interpretation, with numerous worked examples, self- tests and problems. Online Resource CentreFor registered adopters of the book: - Figures and tables of data fTrade ReviewI have never read a book with such a wide scope and coverage. * Dr Paul Gates, University of Bristol *I believe the problem solving approach is absolutely the best way to teach this kind of material. * Professor Russell Howe, University of Aberdeen *Table of ContentsFundamental aspects of characterisation methods in inorganic chemistry Diffraction methods and crystallography Nuclear magnetic resonance Vibrational spectroscopy Electronic absorption and emission spectroscopy X-ray and photoelectron spectroscopy, electron microscopy, and energy dispersive analysis of X-rays Mass spectrometry and chemical and thermal analysis techniques Magnetism Electron paramagnetic resonance spectroscopy Mossbauer spectroscopy and nuclear quadrupole resonance spectroscopy Characterisation of inorganic compounds: example problems with multiple techniques

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Book Synopsis

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Book SynopsisNuclear magnetic resonance (NMR) spectroscopy, a technique widely used for structure determination by chemists and biochemists, is based on the detection of tiny radio signals emitted by the nucleus of an atom when immersed in a strong magnetic field. Every chemical substance gives rise to a recognizable NMR signature closely related to its molecular structure. This comprehensive account adopts an accessible, pictorial approach to teach the fundamental principles of high resolution NMR. Mathematical formalism is used sparingly, and everyday analogies are used to provide insight into the physical behaviour of nuclear spins. The first three chapters set out the basic tools for understanding the rest of the book. Each of the remaining chapters provides a self- contained reference to a specific theme, for example spin echoes, and traces the way it influences our understanding of high resolution NMR methodology. Spin Choreography provides a clear and an authoritative introduction to the funTable of Contents1. Energy levels ; 2. Vector model ; 3. Product operator formalism ; 4. Spin echoes ; 5. Soft radiofrequency pulses ; 6. Separating the wheat from the chaff ; 7. Broadband decoupling ; 8. Two-dimensional spectroscopy ; 9. Nuclear Overhauser effect ; 10. In defence of noise ; 11. Water ; 12. Measurement of coupling constants

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Book SynopsisNuclear Magnetic Resonance offers an accessible introduction to the physical principles of liquid-state NMR, with examples, applications, and exercises provided throughout to enable beginning undergraduates to get to grips with this important analytical technique.Trade ReviewThis book is indisputably a must have for any student, or even teacher, in the field of nuclear magnetic resonance. It is a perfect format for preparing readers for more advanced studies on the topic. Theoretical explanations are illustrated by many examples and applications, and this second edition has been completed with a series of exercises. * Sabine Bouguet-Bonnet, Universite de Lorraine, J. Appl. Cryst. (2017). 50, 1243 *This primer fully deserves to be widely adopted by students (and teachers) of NMR spectroscopy. This book is a complete and very accessible tool for understanding the origin and significance of the basic NMR parameters. * Sabine Bouguet-Bonnet, Universite de Lorraine, J. Appl. Cryst. (2017). 50, 1243 *Table of Contents1. Introduction ; 2. Chemical shifts ; 3. Spin-spin coupling ; 4. Chemical exchange ; 5. Spin relaxation ; 6. NMR experiments

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Book SynopsisThe renowned Oxford Chemistry Primer series, which provides focused introductions to a range of important topics in chemistry, has been refreshed and updated to suit the needs of today''s students, lecturers, and postgraduate researchers. The rigorous, yet accessible, treatment of each subject area is ideal for those wanting a primer in a given topic to prepare them for more advanced study or research. Moreover, cutting-edge examples and applications throughout the texts show the relevance of the chemistry being described to current research and industry. The learning features provided, including questions at the end of every chapter and online multiple-choice questions, encourage active learning and promote understanding. Furthermore, frequent diagrams, margin notes, further reading, and glossary definitions all help to enhance a student''s understanding of these essential areas of chemistry.NMR: The Toolkit describes succinctly the range of NMR techniques commonly used in modern reseTable of ContentsPART A: PRODUCT OPERATORS; PART B: QUANTUM MECHANICS

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Book SynopsisThe renowned Oxford Chemistry Primer series, which provides focused introductions to a range of important topics in chemistry, has been refreshed and updated to suit the needs of today''s students, lecturers, and postgraduate researchers. The rigorous, yet accessible, treatment of each subject area is ideal for those wanting a primer in a given topic to prepare them for more advanced study or research. The learning features provided, including questions at the end of every chapter and online multiple-choice questions, encourage active learning and promote understanding. Moreover, cutting-edge examples and applications throughout the texts show the relevance to current research and industry of the chemistry being described. Electronic Paramagnetic Resonance provides a user-friendly introduction to this powerful tool for characterizing paramagnetic molecules. A versatile technique, EPR is becoming increasingly used across fields as diverse as biology, materials science, chemistry, and physics. This primer provides the perfect introduction to the subject by taking the reader through from basic principles to how spectra can be interpreted in practice, with frequent examples demonstrating the diverse ways in which the technique can be applied.Online Resources The online resources to accompany Electron Paramagnetic Resonance feature: For registered adopters of the text: Figures from the book available to download For students: Full worked solutions to the end-of-chapter exercises Multiple-choice questions for self-directed learningTrade ReviewGood sets of sample spectra to illustrate the underlying principles. * Dr Tien-Sung Tom Lin, Washington University in St. Louis *Combines a sound theoretical basis with a hands-on approach and useful advice for practical work. * Prof. Dr. Gunnar Jeschke, ETH Zürich, Switzerland *Table of Contents1: A brief overview of Electron Paramagnetic Resonance spectroscopy 2: Theory of continuous wave EPR spectroscopy 3: Experimental methods in CW EPR 4: Isotropic EPR spectra of organic radicals 5: Anisotropic EPR spectra in the solid state 6: Transition metal ions and inorganic radicals 7: Systems with multiple unpaired electrons 8: Linewidth of EPR spectra 9: Advanced EPR techniques

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Book SynopsisSpin Dynamics: Basics of Nuclear Magnetic Resonance, Second Edition is a comprehensive and modern introduction which focuses on those essential principles and concepts needed for a thorough understanding of the subject, rather than the practical aspects.Trade Review?What makes this book stand out compared to similar books is the extensive use of pictures and diagrams, which will make this book more appealing to nonphysicists, like chemists and biologists. That this was achieved without loss of rigor is indeed an accomplishment.? ( Doody?s Reviews , November 2009)Table of ContentsPreface. Preface to the First Edition. Introduction. Part 1 Nuclear Magnetism. 1 Matter. 1.1 Atoms and Nuclei. 1.2 Spin. 1.3 Nuclei. 1.4 Nuclear Spin. 1.5 Atomic and Molecular Structure. 1.6 States of Matter. Notes. Further Reading. Exercises. 2 Magnetism. 2.1 The Electromagnetic Field. 2.2 Macroscopic Magnetism. 2.3 Microscopic Magnetism. 2.4 Spin Precession. 2.5 Larmor Frequency. 2.6 Spin-Lattice Relaxation: Nuclear Paramagnetism. 2.7 Transverse Magnetization and Transverse Relaxation. 2.8 NMR Signal. 2.9 Electronic Magnetism. Notes. Further Reading. Exercises. 3 NMR Spectroscopy. 3.1 A Simple Pulse Sequence. 3.2 A Simple Spectrum. 3.4 Relative Spectral Frequencies: Case of Positive Gyromagnetic Ratio. 3.5 Relative Spectral Frequencies: Case of Negative Gyromagnetic Ratio. 3.6 Inhomogeneous Broadening. 3.7 Chemical Shifts. 3.8 J-Coupling Multiplets. 3.9 Heteronuclear Decoupling. Notes. Further Reading. Exercises. Part 2 The NMR Experiment. 4 The NMR Spectrometer. 4.1 The Magnet. 4.2 The Transmitter Section. 4.3 The Duplexer. 4.4 The Probe. 4.5 The Receiver Section. 4.6 Overview of the Radio-Frequency Section. 4.7 Pulsed Field Gradients. Notes. Further Reading. 5 Fourier Transform NMR. 5.1 A Single-Pulse Experiment. 5.2 Signal Averaging. 5.3 Multiple-Pulse Experiments: Phase Cycling. 5.4 Heteronuclear Experiments. 5.5 Pulsed Field Gradient Sequences. 5.6 Arrayed Experiments. 5.7 NMR Signal. 5.8 NMR Spectrum. 5.9 Two-Dimensional Spectroscopy. 5.10 Three-Dimensional Spectroscopy. Part 3 Quantum Mechanics. 6 Mathematical Techniques. 6.1 Functions. 6.2 Operators. 6.3 Eigenfunctions, Eigenvalues and Eigenvectors. 6.4 Diagonalization. 6.5 Exponential Operators. 6.6 Cyclic Commutation. Notes. Further Reading. Exercises. 7 Review of Quantum Mechanics. 7.1 Spinless Quantum Mechanics. 7.2 Energy Levels. 7.3 Natural Units. 7.4 Superposition States and Stationary States. 7.5 Conservation Laws. 7.6 Angular Momentum. 7.7 Spin. 7.8 Spin-1/2. 7.9 Higher Spin. Notes. Further Reading. Exercises. Part 4 Nuclear Spin Interactions. 8 Nuclear Spin Hamiltonian. 8.1 Spin Hamiltonian Hypothesis. 8.2 Electromagnetic Interactions. 8.3 External and Internal Spin Interactions. 8.4 External Magnetic Fields. 8.5 Internal Spin Hamiltonian. 8.6 Motional Averaging. Notes. Further Reading. Exercises. 9 Internal Spin Interactions. 9.1 Chemical Shift. 9.2 Electric Quadrupole Coupling. 9.3 Direct Dipole-Dipole Coupling. 9.4 J-Coupling. 9.5 Spin-Rotation Interaction. 9.6 Summary of the Spin Hamiltonian Terms. Notes. Further Reading. Exercises. Part 5 Uncoupled Spins. 10 Single Spin-1/2. 10.1 Zeeman Eigenstates. 10.2 Measurement of Angular Momentum: Quantum Indeterminacy. 10.3 Energy Levels. 10.4 Superposition States. 10.5 Spin Precession. 10.6 Rotating Frame. 10.7 Precession in the Rotating Frame. 10.8 Radio-Frequency Pulse. Notes. Further Reading. Exercises. 11 Ensemble of Spins-1/2. 11.1 Spin Density Operator. 11.2 Populations and Coherences. 11.3 Thermal Equilibrium. 11.4 Rotating-Frame Density Operator. 11.5 Magnetization Vector. 11.6 Strong Radio-Frequency Pulse. 11.7 Free Precession Without Relaxation. 11.8 Operator Transformations. 11.9 Free Evolution with Relaxation. 11.10 Magnetization Vector Trajectories. 11.11 NMR Signal and NMR Spectrum. 11.12 Single-Pulse Spectra. Notes. Further Reading. Exercises. 12 Experiments on Non-Interacting Spins-1/2. 12.1 Inversion Recovery: Measurement of T1. 12.2 Spin Echoes: Measurement of T2. 12.3 Spin Locking: Measurement of T1ˆ. 12.4 Gradient Echoes. 12.5 Slice Selection. 12.6 NMR Imaging. Notes. Further Reading. Exercises. 13 Quadrupolar Nuclei. 13.1 Spin I = 1. 13.2 Spin I = 3/2. 13.3 Spin I = 5/2. 13.4 Spins I = 7/2. 13.5 Spins I = 9/2. Notes. Further Reading. Exercises. Part 6 Coupled Spins. 14 Spin-1/2 Pairs. 14.1 Coupling Regimes. 14.2 Zeeman Product States and Superposition States. 14.3 Spin-Pair Hamiltonian. 14.4 Pairs of Magnetically Equivalent Spins. 14.5 Weakly Coupled Spin Pairs. Notes. Further Reading. Exercises. 15 Homonuclear AX System. 15.1 Eigenstates and Energy Levels. 15.2 Density Operator. 15.3 Rotating Frame. 15.4 Free Evolution. 15.5 Spectrum of the AX System: Spin-Spin Splitting. 15.6 Product Operators. 15.7 Thermal Equilibrium. 15.8 Radio-Frequency Pulses. 15.9 Free Evolution of the Product Operators. 15.10 Spin Echo Sandwich. Notes. Further Reading. Exercises. 16 Experiments on AX Systems. 16.1 COSY. 16.2 INADEQUATE. 16.3 INEPT. 16.4 Residual Dipolar Couplings. Notes. Further Reading. Exercises. 17 Many-Spin Systems. 17.1 Molecular Spin System. 17.2 Spin Ensemble. 17.3 Motionally Suppressed J-Couplings. 17.4 Chemical Equivalence. 17.5 Magnetic Equivalence. 17.6 Weak Coupling. 17.7 Heteronuclear Spin Systems. 17.8 Alphabet Notation. 17.9 Spin Coupling Topologies. Notes. Further Reading. Exercises. 18 Many-Spin Dynamics. 18.1 Spin Hamiltonian. 18.2 Energy Eigenstates. 18.3 Superposition States. 18.4 Spin Density Operator. 18.5 Populations and Coherences. 18.6 NMR Spectra. 18.7 Many-Spin Product Operators. 18.8 Thermal Equilibrium. 18.9 Radio-Frequency Pulses. 18.10 Free Precession. 18.11 Spin Echo Sandwiches. 18.12 INEPT in an I2S System. 18.13 COSY in Multiple-Spin Systems. 18.14 TOCSY. Notes. Further Reading Exercises. Part 7 Motion and Relaxation. 19 Motion. 19.1 Motional Processes. 19.2 Motional Time-Scales. 19.3 Motional Effects. 19.4 Motional Averaging. 19.5 Motional Lineshapes and Two-Site Exchange. 19.6 Sample Spinning. 19.7 Longitudinal Magnetization Exchange. 19.8 Diffusion. Notes. Further Reading. Exercises. 20 Relaxation. 20.1 Types of Relaxation. 20.2 Relaxation Mechanisms. 20.3 Random Field Relaxation. 20.4 Dipole-Dipole Relaxation. 20.5 Steady-State Nuclear Overhauser Effect. 20.6 NOESY. 20.7 ROESY. 20.8 Cross-Correlated Relaxation. Notes. Further Reading. Exercises. Appendices. Appendix A. A.1 Euler Angles and Frame Transformations. A.2 Rotations and Cyclic Commutation. A.3 Rotation Sandwiches. A.4 Spin-1/2 Rotation Operators. A.5 Quadrature Detection and Spin Coherences. A.6 Secular Approximation. A.7 Quadrupolar Interaction. A.8 Strong Coupling. A.9 J-Couplings and Magnetic Equivalence. A.10 Spin Echo Sandwiches. A.11 Phase Cycling. A.12 Coherence Selection by Pulsed Field Gradients. A.13 Bloch Equations. A.14 Chemical Exchange. A.15 Solomon Equations. A.16 Cross-Relaxation Dynamics. Notes. Further Reading. Appendix B. B.1 Symbols and Abbreviations. B.2 Answers to the Exercises.

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Book SynopsisSpin Dynamics: Basics of Nuclear Magnetic Resonance, Second Edition is a comprehensive and modern introduction which focuses on those essential principles and concepts needed for a thorough understanding of the subject, rather than the practical aspects.Trade Review?What makes this book stand out compared to similar books is the extensive use of pictures and diagrams, which will make this book more appealing to nonphysicists, like chemists and biologists. That this was achieved without loss of rigor is indeed an accomplishment.? ( Doody?s Reviews , November 2009)Table of ContentsPreface. Preface to the First Edition. Introduction. Part 1 Nuclear Magnetism. 1 Matter. 1.1 Atoms and Nuclei. 1.2 Spin. 1.3 Nuclei. 1.4 Nuclear Spin. 1.5 Atomic and Molecular Structure. 1.6 States of Matter. Notes. Further Reading. Exercises. 2 Magnetism. 2.1 The Electromagnetic Field. 2.2 Macroscopic Magnetism. 2.3 Microscopic Magnetism. 2.4 Spin Precession. 2.5 Larmor Frequency. 2.6 Spin-Lattice Relaxation: Nuclear Paramagnetism. 2.7 Transverse Magnetization and Transverse Relaxation. 2.8 NMR Signal. 2.9 Electronic Magnetism. Notes. Further Reading. Exercises. 3 NMR Spectroscopy. 3.1 A Simple Pulse Sequence. 3.2 A Simple Spectrum. 3.4 Relative Spectral Frequencies: Case of Positive Gyromagnetic Ratio. 3.5 Relative Spectral Frequencies: Case of Negative Gyromagnetic Ratio. 3.6 Inhomogeneous Broadening. 3.7 Chemical Shifts. 3.8 J-Coupling Multiplets. 3.9 Heteronuclear Decoupling. Notes. Further Reading. Exercises. Part 2 The NMR Experiment. 4 The NMR Spectrometer. 4.1 The Magnet. 4.2 The Transmitter Section. 4.3 The Duplexer. 4.4 The Probe. 4.5 The Receiver Section. 4.6 Overview of the Radio-Frequency Section. 4.7 Pulsed Field Gradients. Notes. Further Reading. 5 Fourier Transform NMR. 5.1 A Single-Pulse Experiment. 5.2 Signal Averaging. 5.3 Multiple-Pulse Experiments: Phase Cycling. 5.4 Heteronuclear Experiments. 5.5 Pulsed Field Gradient Sequences. 5.6 Arrayed Experiments. 5.7 NMR Signal. 5.8 NMR Spectrum. 5.9 Two-Dimensional Spectroscopy. 5.10 Three-Dimensional Spectroscopy. Part 3 Quantum Mechanics. 6 Mathematical Techniques. 6.1 Functions. 6.2 Operators. 6.3 Eigenfunctions, Eigenvalues and Eigenvectors. 6.4 Diagonalization. 6.5 Exponential Operators. 6.6 Cyclic Commutation. Notes. Further Reading. Exercises. 7 Review of Quantum Mechanics. 7.1 Spinless Quantum Mechanics. 7.2 Energy Levels. 7.3 Natural Units. 7.4 Superposition States and Stationary States. 7.5 Conservation Laws. 7.6 Angular Momentum. 7.7 Spin. 7.8 Spin-1/2. 7.9 Higher Spin. Notes. Further Reading. Exercises. Part 4 Nuclear Spin Interactions. 8 Nuclear Spin Hamiltonian. 8.1 Spin Hamiltonian Hypothesis. 8.2 Electromagnetic Interactions. 8.3 External and Internal Spin Interactions. 8.4 External Magnetic Fields. 8.5 Internal Spin Hamiltonian. 8.6 Motional Averaging. Notes. Further Reading. Exercises. 9 Internal Spin Interactions. 9.1 Chemical Shift. 9.2 Electric Quadrupole Coupling. 9.3 Direct Dipole-Dipole Coupling. 9.4 J-Coupling. 9.5 Spin-Rotation Interaction. 9.6 Summary of the Spin Hamiltonian Terms. Notes. Further Reading. Exercises. Part 5 Uncoupled Spins. 10 Single Spin-1/2. 10.1 Zeeman Eigenstates. 10.2 Measurement of Angular Momentum: Quantum Indeterminacy. 10.3 Energy Levels. 10.4 Superposition States. 10.5 Spin Precession. 10.6 Rotating Frame. 10.7 Precession in the Rotating Frame. 10.8 Radio-Frequency Pulse. Notes. Further Reading. Exercises. 11 Ensemble of Spins-1/2. 11.1 Spin Density Operator. 11.2 Populations and Coherences. 11.3 Thermal Equilibrium. 11.4 Rotating-Frame Density Operator. 11.5 Magnetization Vector. 11.6 Strong Radio-Frequency Pulse. 11.7 Free Precession Without Relaxation. 11.8 Operator Transformations. 11.9 Free Evolution with Relaxation. 11.10 Magnetization Vector Trajectories. 11.11 NMR Signal and NMR Spectrum. 11.12 Single-Pulse Spectra. Notes. Further Reading. Exercises. 12 Experiments on Non-Interacting Spins-1/2. 12.1 Inversion Recovery: Measurement of T1. 12.2 Spin Echoes: Measurement of T2. 12.3 Spin Locking: Measurement of T1ˆ. 12.4 Gradient Echoes. 12.5 Slice Selection. 12.6 NMR Imaging. Notes. Further Reading. Exercises. 13 Quadrupolar Nuclei. 13.1 Spin I = 1. 13.2 Spin I = 3/2. 13.3 Spin I = 5/2. 13.4 Spins I = 7/2. 13.5 Spins I = 9/2. Notes. Further Reading. Exercises. Part 6 Coupled Spins. 14 Spin-1/2 Pairs. 14.1 Coupling Regimes. 14.2 Zeeman Product States and Superposition States. 14.3 Spin-Pair Hamiltonian. 14.4 Pairs of Magnetically Equivalent Spins. 14.5 Weakly Coupled Spin Pairs. Notes. Further Reading. Exercises. 15 Homonuclear AX System. 15.1 Eigenstates and Energy Levels. 15.2 Density Operator. 15.3 Rotating Frame. 15.4 Free Evolution. 15.5 Spectrum of the AX System: Spin-Spin Splitting. 15.6 Product Operators. 15.7 Thermal Equilibrium. 15.8 Radio-Frequency Pulses. 15.9 Free Evolution of the Product Operators. 15.10 Spin Echo Sandwich. Notes. Further Reading. Exercises. 16 Experiments on AX Systems. 16.1 COSY. 16.2 INADEQUATE. 16.3 INEPT. 16.4 Residual Dipolar Couplings. Notes. Further Reading. Exercises. 17 Many-Spin Systems. 17.1 Molecular Spin System. 17.2 Spin Ensemble. 17.3 Motionally Suppressed J-Couplings. 17.4 Chemical Equivalence. 17.5 Magnetic Equivalence. 17.6 Weak Coupling. 17.7 Heteronuclear Spin Systems. 17.8 Alphabet Notation. 17.9 Spin Coupling Topologies. Notes. Further Reading. Exercises. 18 Many-Spin Dynamics. 18.1 Spin Hamiltonian. 18.2 Energy Eigenstates. 18.3 Superposition States. 18.4 Spin Density Operator. 18.5 Populations and Coherences. 18.6 NMR Spectra. 18.7 Many-Spin Product Operators. 18.8 Thermal Equilibrium. 18.9 Radio-Frequency Pulses. 18.10 Free Precession. 18.11 Spin Echo Sandwiches. 18.12 INEPT in an I2S System. 18.13 COSY in Multiple-Spin Systems. 18.14 TOCSY. Notes. Further Reading Exercises. Part 7 Motion and Relaxation. 19 Motion. 19.1 Motional Processes. 19.2 Motional Time-Scales. 19.3 Motional Effects. 19.4 Motional Averaging. 19.5 Motional Lineshapes and Two-Site Exchange. 19.6 Sample Spinning. 19.7 Longitudinal Magnetization Exchange. 19.8 Diffusion. Notes. Further Reading. Exercises. 20 Relaxation. 20.1 Types of Relaxation. 20.2 Relaxation Mechanisms. 20.3 Random Field Relaxation. 20.4 Dipole-Dipole Relaxation. 20.5 Steady-State Nuclear Overhauser Effect. 20.6 NOESY. 20.7 ROESY. 20.8 Cross-Correlated Relaxation. Notes. Further Reading. Exercises. Appendices. Appendix A. A.1 Euler Angles and Frame Transformations. A.2 Rotations and Cyclic Commutation. A.3 Rotation Sandwiches. A.4 Spin-1/2 Rotation Operators. A.5 Quadrature Detection and Spin Coherences. A.6 Secular Approximation. A.7 Quadrupolar Interaction. A.8 Strong Coupling. A.9 J-Couplings and Magnetic Equivalence. A.10 Spin Echo Sandwiches. A.11 Phase Cycling. A.12 Coherence Selection by Pulsed Field Gradients. A.13 Bloch Equations. A.14 Chemical Exchange. A.15 Solomon Equations. A.16 Cross-Relaxation Dynamics. Notes. Further Reading. Appendix B. B.1 Symbols and Abbreviations. B.2 Answers to the Exercises.

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Book SynopsisThis text is aimed at people who have some familiarity with high-resolution NMR and who wish to deepen their understanding of how NMR experiments actually work'. This revised and updated edition takes the same approach as the highly-acclaimed first edition. The text concentrates on the description of commonly-used experiments and explains in detail the theory behind how such experiments work. The quantum mechanical tools needed to analyse pulse sequences are introduced set by step, but the approach is relatively informal with the emphasis on obtaining a good understanding of how the experiments actually work. The use of two-colour printing and a new larger format improves the readability of the text. In addition, a number of new topics have been introduced: How product operators can be extended to describe experiments in AX2 and AX3 spin systems, thus making it possible to discuss the important APT, INEPT and DEPT experiments often used in carbon-13 NMR. SpTable of ContentsPreface v Preface to the first edition vi 1 What this book is about and who should read it 1 1.1 How this book is organized 2 1.2 Scope and limitations 3 1.3 Context and further reading 3 1.4 On-line resources 4 1.5 Abbreviations and acronyms 4 2 Setting the scene 5 2.1 NMR frequencies and chemical shifts 5 2.2 Linewidths, lineshapes and integrals 9 2.3 Scalar coupling 10 2.4 The basic NMR experiment 13 2.5 Frequency, oscillations and rotations 15 2.6 Photons 20 2.7 Moving on 21 2.8 Further reading 21 2.9 Exercises 22 3 Energy levels and NMR spectra 23 3.1 The problem with the energy level approach 24 3.2 Introducing quantum mechanics 26 3.3 The spectrum from one spin 31 3.4 Writing the Hamiltonian in frequency units 34 3.5 The energy levels for two coupled spins 35 3.6 The spectrum from two coupled spins 38 3.7 Three spins 40 3.8 Summary 44 3.9 Further reading 44 3.10 Exercises 45 4 The vector model 47 4.1 The bulk magnetization 47 4.2 Larmor precession 50 4.3 Detection 51 4.4 Pulses 52 4.5 On-resonance pulses 57 4.6 Detection in the rotating frame 60 4.7 The basic pulse–acquire experiment 60 4.8 Pulse calibration 61 4.9 The spin echo 63 4.10 Pulses of different phases 66 4.11 Off-resonance effects and soft pulses 67 4.12 Moving on 71 4.13 Further reading 71 4.14 Exercises 72 5 Fourier transformation and data processing 77 5.1 How the Fourier transform works 78 5.2 Representing the FID 82 5.3 Lineshapes and phase 83 5.4 Manipulating the FID and the spectrum 90 5.5 Zero filling 99 5.6 Truncation 100 5.7 Further reading 101 5.8 Exercises 102 6 The quantum mechanics of one spin 105 6.1 Introduction 105 6.2 Superposition states 106 6.3 Some quantum mechanical tools 107 6.4 Computing the bulk magnetization 112 6.5 Summary 117 6.6 Time evolution 118 6.7 RF pulses 123 6.8 Making faster progress: the density operator 126 6.9 Coherence 134 6.10 Further reading 135 6.11 Exercises 136 7 Product operators 139 7.1 Operators for one spin 139 7.2 Analysis of pulse sequences for a one-spin system 143 7.3 Speeding things up 146 7.4 Operators for two spins 149 7.5 In-phase and anti-phase terms 152 7.6 Hamiltonians for two spins 157 7.7 Notation for heteronuclear spin systems 157 7.8 Spin echoes and J-modulation 158 7.9 Coherence transfer 166 7.10 The INEPT experiment 167 7.11 Selective COSY 171 7.12 Coherence order and multiple-quantum coherences 173 7.13 Summary 178 7.14 Further reading 179 7.15 Exercises 180 8 Two-dimensional NMR 183 8.1 The general scheme for two-dimensional NMR 184 8.2 Modulation and lineshapes 187 8.3 COSY 190 8.4 DQF COSY 200 8.5 Double-quantum spectroscopy 203 8.6 Heteronuclear correlation spectra 208 8.7 HSQC 209 8.8 HMQC 212 8.9 Long-range correlation: HMBC 215 8.10 HETCOR 220 8.11 TOCSY 221 8.12 Frequency discrimination and lineshapes 226 8.13 Further reading 236 8.14 Exercises 238 9 Relaxation and the NOE 241 9.1 The origin of relaxation 242 9.2 Relaxation mechanisms 249 9.3 Describing random motion – the correlation time 251 9.4 Populations 258 9.5 Longitudinal relaxation behaviour of isolated spins 263 9.6 Longitudinal dipolar relaxation of two spins 267 9.7 The NOE 274 9.8 Transverse relaxation 286 9.9 Homogeneous and inhomogeneous broadening 300 9.10 Relaxation due to chemical shift anisotropy 304 9.11 Cross correlation 306 9.12 Summary 311 9.13 Further reading 311 9.14 Exercises 313 10 Advanced topics in two-dimensional NMR 319 10.1 Product operators for three spins 320 10.2 COSY for three spins 325 10.3 Reduced multiplets in COSY spectra 330 10.4 Polarization operators 337 10.5 ZCOSY 345 10.6 HMBC 347 10.7 Sensitivity-enhanced experiments 349 10.8 Constant time experiments 353 10.9 TROSY 358 10.10 Double-quantum spectroscopy of a three-spin system 366 10.11 Further reading 374 10.12 Exercises 376 11 Coherence selection: phase cycling and field gradient pulses 381 11.1 Coherence order 382 11.2 Coherence transfer pathways 387 11.3 Frequency discrimination and lineshapes 389 11.4 The receiver phase 391 11.5 Introducing phase cycling 395 11.6 Some phase cycling ‘tricks’ 401 11.7 Axial peak suppression 403 11.8 CYCLOPS 403 11.9 Examples of practical phase cycles 404 11.10 Concluding remarks about phase cycling 408 11.11 Introducing field gradient pulses 409 11.12 Features of selection using gradients 416 11.13 Examples of using gradient pulses 421 11.14 Advantages and disadvantages of coherence selection with gradients 426 11.15 Suppression of zero-quantum coherence 426 11.16 Selective excitation with the aid of gradients 432 11.17 Further reading 435 11.18 Exercises 436 12 Equivalent spins and spin system analysis 441 12.1 Strong coupling in a two-spin system 442 12.2 Chemical and magnetic equivalence 446 12.3 Product operators for AXn (InS) spin systems 450 12.4 Spin echoes in InS spin systems 455 12.5 INEPT in InS spin systems 458 12.6 DEPT 462 12.7 Spin system analysis 468 12.8 Further reading 477 12.9 Exercises 478 13 How the spectrometer works 483 13.1 The magnet 483 13.2 The probe 485 13.3 The transmitter 486 13.4 The receiver 488 13.5 Digitizing the signal 489 13.6 Quadrature detection 491 13.7 The pulse programmer 493 13.8 Further reading 493 13.9 Exercises 494 A Some mathematical topics 495 A.1 The exponential function and logarithms 495 A.2 Complex numbers 497 A.3 Trigonometric identities 499 A.4 Further reading 500 Index 501

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Book SynopsisThe content of this volume has been added to eMagRes (formerly Encyclopedia of Magnetic Resonance) - theTable of ContentsContributors ix Series Preface xiii Volume Preface xv Part A: Surface Coils 1 1 An Historical Introduction to Surface Coils: The Early Days 3 Joseph J. H. Ackerman 2 Radiofrequency Coils for NMR: A Peripatetic History of Their Twists and Turns 9 Eiichi Fukushima 3 Quadrature Surface Coils 17 Christopher M. Collin and, Andrew G. Webb 4 Double-Tuned Surface Coils 27 Barbara L. Beck 5 Nested Surface Coils for Multinuclear NMR 39 Arthur W. Magill and Rolf Gruetter 6 Quadrature Transverse Electromagnetic (TEM) Surface Coils 51 Nikolai I. Avdievich Part B: Array Coils 63 7 Receiver Loop Arrays 65 Steven M. Wright 8 Coil Array Design for Parallel Imaging: Theory and Applications 81 Daniel K. Sodickson, Michael A. Ohliger, Riccardo Lattanzi and Graham C. Wiggins 9 Transceiver Loop Arrays 101 Randy Duensing 10 Characterization of Multichannel Coil Arrays on the Benchtop 111 Mark A Griswold Part C: Volume Coils 121 11 Birdcage Volume Coil Design 123 Nicola De Zanche 12 Double-Tuned Birdcage Coils: Construction and Tuning 137 Joseph Murphy-Boesch 13 TEM Body Coils 147 J. Thomas Vaughan 14 TEM Transceiver Head Array Coils for Ultra High Magnetic Fields 169 Gregor Adriany 15 TEM Arrays, Design and Implementation 175 Carl Snyder 16 Transverse Electromagnatic (TEM) Coils for Extremities 185 Nikolai I. Avdievich 17 Antennas as Surface Array Elements for Body Imaging at Ultra-high Field Strengths 197 A. J. E. Raaijmakers and C. A. T. van den Berg Part D: Special Purpose Coils 209 18 Catheter Coils 211 Ergin Atalar 19 Microcoils 225 Andrew G. Webb 20 Cryogenic and Superconducting Coils for MRI 233 Sven Junge 21 Litz Coils for High Resolution and Animal Probes, Especially for Double Resonance 245 F. David Doty, George Entzminger Jr 22 Millipede Coils 259 Ernest W. H. Wong Part E: Coil Interface Circuits 269 23 Receiver Design for MR 271 David I. Hoult 24 Radiofrequency Power Amplifiers for NMR and MRI 299 Daniel P. Myer 25 Impedance Matching and Baluns 315 David M. Peterson Part F: Coil Modeling and Evaluation 325 26 Radiofrequency MRI Coil Analysis: A Standard Procedure 327 Rostislav A. Lemdiasov, Reinhold Ludwig 27 Practical Electromagnetic Modeling Methods 339 Jian-Ming Jin 28 Radiofrequency Fields and SAR for Bird Cages 363 Tamer S. Ibrahim 29 RF Field Modeling for Double-Tuned Volume Coils 377 Wanzhan Liu 30 Radiofrequency Fields and SAR for Transverse Electromagnetic (TEM) Surface Coils 387 Can Eyup Akgun 31 TEM Coil Fields and SAR 397 Jinfeng Tian Part G: RF Safety 407 32 RF Device Safety and Compatibility 409 John Nyenhuis 33 Radiofrequency Heating Models and Measurements Devashish Shrivastava, J. Thomas Vaughan 425 Index 437

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Book SynopsisThis volume covers the new methodological advances in NMR spectroscopy that have been developed since the publication of the first edition. These include: ''indirect detection'' methods, particularly proton-detected carbon-13 spectra, which have profoundly increased NMR sensitivities; 3- and even higher- dimensional NMR methods which have further increased spectral resolving and correlating power; powerful new computer programs which assist in all phases of data analysis and ultimately make possible rigorous interpretations of complex 2D and higher- dimensional NMR spectra using molecular mechanics and dynamics calculations; and field gradient technology which makes it possible to acquire 2D and higher-dimensional spectra of concentrated samples very rapidly, greatly reducing experiment times. This new edition retains the original format of the first edition with introductory chapters covering descriptions, basic theoretical treatments and experimental aspects of the methods. These areTable of ContentsFrom the Contents: Introduction to Multi-Dimensional NMR Methods/ Experimental Aspects of Two-Dimensional NMR/ Proton Detected Heteronuclear and Multi-Dimensional NMR/ Computer-Aided Analysis of Multi-Dimensional NMR Spectra/ NMR of Pesticides/ Protein Structure Calculation Using NMR Restraints/ Studies of Nucleic Acid Structures Based on NMR Results/ Two-Dimensional and Related NMR Methods in Structural Analysis of Oligo- and Polysaccharides/ Steroid Structural Analysis of Two-Dimensional NMR/ Applications of Two-Dimensional NMR to the Characterization of Synthetic Organic Materials/ Two-Dimensional NMR in Natural Products and Pharmaceutical Chemistry

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Book SynopsisDynamic Spin Chemistry Edited by Saburo Nagakura, Hisaharu Hayashi and Tohru Azumi Because of increasing concerns over the effects of electromagnetic radiation on the human body, it has become essential to understand how chemical and biological reactions are affected by magnetic fields. Dynamic Spin Chemistry focuses on theoretical and experimental research showing the great influence on the dynamic behavior of molecules due to external magnetic fields, such as magnetic quenching of gaseous fluorescence, effects on chemical reaction rates and chemically induced dynamic nuclear and electron polarization. This book discusses both the theoretical and experimental foundations of dynamic spin chemistry, as well as its future trends. After the introductory chapter, the next three chapters discuss magnetic field effects and magnetic isotope effects on chemical reactions in solution and on the dynamic behavior of excited molecules in the gas phase. Subsequent chapters deal with the effects on Table of ContentsWhat is Dynamic Spin Chemistry? Magnetic Field and Magnetic Isotope Effects on Reactions of Radical Pairs. Magnetic Field and Magnetic Isotope Effects on Biradical Reactions. Magnetic Field Effects on Dynamic Behavior of Excited Molecules in the Gas Phase. Magnetic Field Effects on Chemical Equilibria. Spin Spectroscopy Focusing on Nuclear Spin Polarization. Chemically Induced Dynamic Electron Polarization (CIDEP) Studies in Photochemical Reactions. Reaction-Yield-Detected ESR and Its Application to Control Chemical Reactions. Index.

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Book SynopsisOne of the most outstanding contributions of NMR to chemistry concerns the information which can be obtained at the molecular level as a result of the time-dependence of NMR spectra. The importance of this information is well illustrated by the large number of applications which have resulted from research in this field. To date, however, both the theory and its applications have only been available in widely scattered articles in the literature. Dynamics of Solutions and Fluid Mixtures by NMR is the first single volume giving a comprehensive coverage of time-dependent effects in NMR, and of the information which can be obtained by investigation of these phenomena. The ten chapters, all written by acknowledged experts in their respective fields, are arranged in a logical progression. The first three chapters give an overview of NMR spectroscopy and the fundamental aspects of molecular dynamics. Topics covered in later chapters include specific relaxation mechanisms, the use of field grTable of ContentsTimescales in NMR: Relaxation Phenomena in Relation with MolecularReorientation (D. Canet & J. Robert). Timescales in NMR: Nuclear Site Exchange and Dynamic NMR(J.-J. Delpuech). Nuclear Paramagnetic Spin Relaxation Theory: Paramagnetic SpinProbes in Homogeneous and Microheterogeneous Solutions (P.Westlund). Quadrupolar Probes in Solution (J. Grandjean & P.Laszlo). Solvent Exchange on Metal Ions: A Variable Pressure NMR Approach(U. Frey, et al.). Applications of Field Gradients in NMR (D. Canet & M.Decorps). Surfactant Solutions: Aggregation Phenomena and Microheterogeneity(B. Lindman, et al.). Polymers and Biopolymers in the Liquid State (M.Krajewski-Bertrand, et al.). Liquid-Like Molecules in Rigid Matrices and in Soft Matter (J.Cohen-Addad, et al.). Index.

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Book SynopsisThis book is for those familiar with solution-state NMR who are encountering solid-state NMR for the first time. It presents the current understanding and applications of solid-state NMR with a rigorous but readable approach, making it easy for someone who merely wishes to gain an overall impression of the subject without details.Table of ContentsList of Contributors. Preface. Acknowledgements. Part I - The Theory of Solid-State NMR and its Experiments. 1. The Basics of Solid-State NMR. 2. Essential Techniques for Spin-1/2 Nuclei. 3. Dipolar Coupling - its Measurements and Uses. 4. Quadrupolar Coupling - its Measurements and Uses. 5. Shielding and Chemical Shift. Part II - Applications of Solid-state NMR. 6. NMR Techniques for Studying Molecular Motion in Solids. 7. Molecular Structure Determination: Applications in Biology. 8. NMR Studies of Oxide Glass Structure. 9. Porous Materials. 10. Solid Polymers. 11. Liquid-Crystalline Materials. References. Index.

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Book SynopsisMagnetic resonance has long demonstrated its tremendous versatility in many areas of science. Nowhere has this been more apparent than in food science, where problems encountered in a variety of situations can be resolved using one of the many techniques available to the magnetic resonance practitioner. From structural studies and investigations of molecules in frozen sugar solutions, to identifying the origins of salmon and detecting free radicals in irradiated food, magnetic resonance techniques can provide useful information. Divided into four sections entitled A View Towards the Next Century; Food Safety and Health; Structure and Dynamics; and Analysis, Monitoring and Authentication, the book consists of top quality contributions from renowned international scientists, and looks at what magnetic resonance techniques can offer both now and in the future. Offering state-of-the-art material, Magnetic Resonance in Food Science: A View to the Future is essential reading for both academiTrade Review"... a valuable addition to the literature. It should be of great use in research, tertiary education and industrial situations and is highly recommended." * Food Australia, 55, (1, 2) January/February 2003, p 53 *Table of ContentsA View Towards The Next Century; Food Safety and Health; Structure and Dynamics; Analysis, Monitoring and Authentication; Subject Index.

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Book SynopsisCombines clear and concise discussions of key NMR concepts with succinct and illustrative examples Designed to cover a full course in Nuclear Magnetic Resonance (NMR) Spectroscopy, this text offers complete coverage of classic (one-dimensional) NMR as well as up-to-date coverage of two-dimensional NMR and other modern methods. It contains practical advice, theory, illustrated applications, and classroom-tested problems; looks at such important ideas as relaxation, NOEs, phase cycling, and processing parameters; and provides brief, yet fully comprehensible, examples. It also uniquely lists all of the general parameters for many experiments including mixing times, number of scans, relaxation times, and more. Nuclear Magnetic Resonance Spectroscopy: An Introduction to Principles, Applications, and Experimental Methods, 2nd Edition begins by introducing readers to NMR spectroscopy - an analytical technique used in modern chemistry, biochemistry, and biology tTable of ContentsPreface to First Edition Preface to Second Edition Symbols Abbreviations 1. Introduction 1.1. Magnetic Properties of Nuclei 1.2. The Chemical Shift 1.3. Excitation and Relaxation 1.4. Pulsed Experiments 1.5. The Coupling Constant 1.6. Quantitation and Complex Splitting 1.7. Commonly Studied Nuclides 1.8. Dynamic Effects 1.9. Spectra of Solids Problems Tips on Solving NMR Problems Bibliography 2. Introductory Experimental Methods 2.1. The Spectrometer 2.2. Sample Preparation 2.3. Optimizing the Signal 2.3a. Sample Tube Placement 2.3b. Probe Tuning 2.3c. Field/Frequency Locking 2.3d. Spectrometer Shimming 2.4. Determination of NMR Spectra-Acquisition Parameters 2.4a. Number of Data Points 2.4b. Spectral Width 2.4c. Filter Bandwidth 2.4d. Acquisition Time 2.4e. Transmitter Offset 2.4f. Flip Angle 2.4g. Receiver Gain 2.4h. Number of Scans 2.4i. Steady-State Scans 2.4j. Oversampling and Digital Filtration 2.4k. Decoupling for X Nuclei 2.4l. Typical NMR Experiments 2.5. Determination of NMR Spectral-Processing Parameters 2.5a. Exponential Weighting 2.5b. Zero Filling 2.5c. FID Truncation and Spectral Artifacts 2.5d. Resolution 2.6. Determination of NMR Spectra: Spectral Presentation 2.6a. Signal Phasing and Baseline Correction 2.6b. Zero Referencing 2.6c. Determination of Certain NMR Parameters 2.7. Calibrations 2.7a. Pulse Width (Flip Angle) 2.8b. Decoupler Field Strength Problems Bibliography 3. The Chemical Shift 3.1. Factors That Influence Proton Shifts 3.2. Proton Chemical Shifts and Structure 3.2a. Saturated Aliphatics 3.2b. Unsaturated Aliphatics 3.2c. Aromatics 3.2d. Protons on Oxygen and Nitrogen 3.2e. Programs for Empirical Calculations 3.3. Medium and Isotope Effects 3.4. Factors That Influence Carbon Shifts 3.5. Carbon Chemical Shifts and Structure 3.5a. Saturated Aliphatics 3.5b. Unsaturated Compounds 3.5c. Carbonyl Groups 3.5d. Programs for Empirical Calculation 3.6. Tables of Chemical Shifts Problems Further Tips on Solving NMR Problems Bibliography 4. The Coupling Constant 4.1. First- and Second-Order Effects 4.2. Chemical and Magnetic Equivalence 4.3. Signs and Mechanisms of Coupling 4.4. Couplings over One Bond 4.5. Geminal Couplings 4.6. Vicinal Couplings 4.7. Long-Range Couplings 4.8. Spectral Analysis 4.9. Tables of Coupling Constants Problems Bibliography 5. Further Topics in One-Dimensional NMR Spectroscopy 5.1. Spin-Lattice and Spin-Spin Relaxation 5.2. Reactions on the NMR Time Scale 5.3. Multiple Resonance 5.4. The Nuclear Overhauser Effect 5.5. Spectral Editing 5.6. Sensitivity Enhancement 5.7. Carbon Connectivity 5.8. Phase Cycling, Composite Pulses, and Shaped Pulses Problems Bibliography 6. Two-Dimensional NMR Spectroscopy 6.1. Proton-Proton Correlation Through J Coupling 6.2. Proton-Heteronucleus Correlation 6.3. Proton-Proton Correlation Through Space or Chemical Exchange 6.4. Carbon-Carbon Correlation 6.5. Higher Dimensions 6.6. Pulsed Field Gradients 6.7. Diffusion-Ordered Spectroscopy 6.7. Summary of Two-Dimensional Methods Problems Bibliography 7. Advanced Experimental Methods Part A. One-Dimensional Techniques 7.1. T1 Measurements 7.2. 13C Spectral Editing Experiments 7.2a. The APT Experiment 7.2b. The DEPT Experiment 7.3. NOE Experiments 7.3a. The NOE Difference Experiment 7.3b. The Double-Pulse, Field-Gradient, Spin-Echo NOE Experiment Part B. Two-Dimensional Techniques 7.4. Two-Dimensional NMR Data-Acquisition Parameters 7.4a. Number of Data Points 7.4b. Number of Time Increments 7.4c. Spectral Widths 7.4d. Acquisition Time 7.4e. Transmitter Offset 7.4f. Flip Angle 7.4g. Relaxation Delay 7.4h. Receiver Gain 7.4i. Number of Scans per Time Increment 7.4j. Steady-State Scans 7.5. Two-Dimensional NMR Data-Processing Parameters 7.5a. Weighting Functions 7.5b. Zero Filling 7.5c. Digital Resolution 7.5d. Linear Prediction 7.6. Two-Dimensional NMR Data Display 7.6a. Phasing and Zero Referencing 7.6b. Symmetrization 7.6c. Use of Cross Sections in Analysis Part C. Two-Dimensional Techniques: The Experiments 7.7. Homonuclear Chemical-Shift Correlation Experiments via Scalar Coupling 7.7a. The COSY Family: COSY-90°, COSY-45°, Long-Range COSY, and DQF-COSY 7.7b. The TOCSY Experiment 7.8. Direct Heteronuclear Chemical-Shift Correlation via Scalar Coupling 7.8a. The HMQC Experiment 7.8b. The HSQC Experiment 7.8c. The HETCOR Experiment 7.9. Indirect Heteronuclear Chemical-Shift Correlation via Scalar Coupling 7.9a. The HMBC Experiment 7.9b. The FLOCK Experiment 7.9c. The HSQC-TOCSY Experiment 7.10. Homonuclear Chemical-Shift Correlation via Dipolar Coupling 7.10a. The NOESY Experiment 7.10b. The ROESY Experiment 7.11. 1D and Advanced 2D Experiments 7.11a. The 1D TOCSY Experiment 7.11b. The 1D NOESY and ROESY Experiments 7.11c. The Multiplicity-Edited HSQC Experiment 7.11d. The H2BC Experiment 7.11e. Nonuniform Sampling 7.11f. Pure Shift NMR 7.11g. Covariance NMR 7.12. Pure Shift-Covariance NMR Bibliography 8. Structural Elucidation: An Example Part A. Spectral Analysis 8.1. 1H NMR Data 8.2. 13C NMR Data 8.3. The DEPT Experiment 8.4. The HSQC Experiment 8.5. The COSY Experiment 8.6. The HMBC Experiment 8.7. General Molecular Assembly Strategy 8.8. A Specific Molecular Assembly Procedure 8.9. The NOESY Experiment Part B Computer-Assisted Structure Elucidation 8.10. CASE Procedures 8.11. T-2 Toxin Appendix 1 Derivation of the NMR Equation Appendix 2 The Bloch Equations Appendix 3 Quantum Mechanical Treatment of the Two-Spin System Appendix 4 Analysis of Second-Order, Three- and Four-Spin Systems by Inspection Appendix 5 Relaxation Appendix 6 Product-Operator Formalism and Coherence-Level Diagrams Bibliography Appendix 7 Stereochemical Considerations A7.1. Homotopic Groups A7.2. Enantiotopic Groups A7.3. Diastereotopic Groups Bibliography Index

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Book SynopsisCovers 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.Trade Review"Overall this is an excellent book and one that I personally will find very useful. I will recommend it to my postgraduate students and prostdoctoral research fellows for its detailed and careful explanations of a wide range of experimental methods in solid-state NMR spectroscopy." "The book is clear and straightforward...the level of detail is very impressive and the author does not shirk her duty to explain some of the most notoriously difficult concepts in this area." Chemistry World, Vol 2, No 1, January 2005 "The theoretical approaches, the description of methods and the demonstration of the applications are clearly given in this book, which can be recommended to students and researchers in physical, analytical and organic chemistry and also biology who need access to solid-state NMR for the characterization of structures and dynamics of chemical or biological compounds.” Magnetic Resonance in Chemistry, 2004, vol 42Table of ContentsPreface, 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 ˆ ∆ 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

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Book SynopsisDescribing comprehensively the development and applications of NMR to oil and gas exploration, this book will bring the literature up to date as it has developed very quickly in the last two decades. Outlining new methodologies, it will provide a thorough and comprehensive document enabling a better understanding of the basics of NMR physics, petrophysics, downhole tools and data interpretation. Written by an author with more than 30 years’ experience in this hot and important topic, this book is designed to meet the needs of the community and encourage applications in low field NMR.Table of ContentsOverview of Borehole NMR in Oil and Applications; Fundamentals of NMR Physics; Fundamentals of NMR Petrophysics and Fluids Typing; Principles of Borehole NMR Tools; Fundamentals of Borehole NMR Data Processing and Inversion; Downhole NMR Stand-alone Analysis; Integration of NMR With Other Logs; NMR Log Quality Control; Borehole NMR Job Planning; Core Analysis Supports Borehole NMR Applications

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Book SynopsisThis textbook is designed for graduate students to introduce the basic concepts of Nuclear Magnetic Resonance spectroscopy (NMR), spectral analysis and modern developments such as multidimensional NMR, in reasonable detail and rigor. The book is self-contained, so, a unique textbook in that sense with end of chapter exercises included supported by a solution manual. Some of the advanced topics are included as Appendices for quick reference. Students of chemistry who have some exposure to mathematics and physics will benefit from this book and it will prepare them to pursue research in different branches of Chemistry or Biophysics or Structural Biology.​Table of ContentsChapter-1: BASIC CONCEPTS 1.1 Nuclear Spin and Magnetic Moments 1.2 Nuclear Spins in a Magnetic Field 1.3 Spin Lattice Relaxation 1.4 Spin temperature 1.5 Resonance Absorption of Energy and The NMR Experiment 1.5.1. The basic NMR spectrometer 1.6 Kinetics of Resonance Absorption 1.7 Selection Rules 1.8 Line widths 1.9 Bloch equations 1.10 More about relaxation 1.11 Sensitivity EXERCISES CHAPTER 2: HIGH RESOLUTION NMR SPECTRA OF MOLECULES 2.1 Introduction 2.2 Chemical Shift 2.2.1 Anisotropy of chemical shifts 2.2.2 Factors Influencing Isotropic Chemical shifts 2.3 Spin-Spin Coupling 2.4 Analysis of NMR spectra of molecules 2.4.1 First Order Analysis 2.4.2 Quantum Mechanical Analysis 2.5 Dynamic Effects in the NMR spectra 2.5.1 Two site Chemical Exchange 2.5.2. Collapse of spin multiplets 2.5.3 Conformational Averaging of J- values EXERCISES CHAPTER 3: FOURIER TRANSFORM NMR 3.1 Introduction 3.2 Principles of Fourier transform NMR 3.3 Theorems on Fourier transforms 3.4 The FTNMR Spectrometer 3.5. Practical aspects of recording FTNMR spectra 3.5.1. Carrier Frequency and off-set 3.5.2. RF pulse 3.5.3. Free Induction Decay (FID) and the spectrum 3.5.4. Single channel and quadrature detection 3.5.5. Signal digitization and sampling 3.5.6. Folding of signals 3.5.7. Acquisition time and the resolution 3.5.8. Signal averaging and Pulse repetition rate 3.6. Data processing in FT NMR 3.6.1. Zero filling 3.6.2. Digital filtration or window multiplication or apodization 3.7 Phase correction 3.8. Dynamic range in FTNMR 3.9. Spin-echo 3.10. Measurement of relaxation times 3.10.1. Measurement of relaxation time 3.10.2. Measurement of relaxation time 3.11. Water suppression through spin-echo: Watergate 3.12 Spin decoupling 3.13 Broad band decoupling 3.14 Biliniear Rotational Decoupling (BIRD) EXERCISES CHAPTER 4: POLARIZATION TRANSFER 4.1 Introduction 4.2 Experimental Schemes 4.3 Origin of NOE 4.3.1 A simplified treatment 4.3.2 A more rigorous treatment 4.4 Steady state NOE 4.5 Transient NOE 4.6. Selective population inversion 4.7. INEPT 4.7.1. Disadvantages of INEPT 4.8 Refocused INEPT 4.9 DEPT EXERCISES CHAPTER 5: Density matrix description of NMR 5.1 Introduction 5.2 Density matrix 5.3 Elements of Density Matrix 5.4. Time evolution of density operator 5.5. Matrix representations of RF pulses 5.6. Product Operator Formalism 5.6.1. Basis operator sets 5.6.2. Time-evolution of Cartesian Basis Operators 5.6.2.1 Free evolution under the influence of the Hamiltonian 5.6.2.2 Chemical Shift evolution 5.6.2.3 Scalar coupling evolution 5.6.2.4 Rotation by pulses 5.6.2.5 Calculation of the spectrum of J-coupled two spin system EXERCISES Chapter 6: Multidimensional NMR Spectroscopy 6.1 Segmentation of the time axis 6.2 Two dimensional NMR 6.3 Two-dimensional Fourier Transformation in NMR 6.4 Peak shapes in 2D spectrum 6.5 Quadrature detection in two-dimensional NMR 6.6 Types of 2D-NMR spectra 6.6.1 2D- resolution/ separation experiments 6.6.2. Two-dimensional correlation experiments 6.6.2.1 The COSY experiment 6.6.2.1.1 COSY of two-spins 6.6.2.1.2 COSY of three-spins 6.6.2.1.3 Disadvantages of COSY 6.6.2.2 Double-Quantum Filtered COSY (DQF-COSY) 6.6.2.3 Total Correlation Spectroscopy (TOCSY) 6.6.2.4 Two-dimensional Nuclear Overhauser Effect spectroscopy (2D-NOESY) 6.6.2.5 Two-dimensional ROESY 6.6.3 Two-dimensional heteronuclear correlation experiments 6.6.3.1 Heteronuclear COSY 6.6.3.2 Heteronuclear Multiple Bond Correlation (HMBC) 6.6.3.3 Combination of mixing sequences 6.7 Three dimensional NMR 6.7.1 The CT-HNCA experiment 6.7.2 The HNN experiment 6.7.3 The constant-time HN(CO)CA experiment 6.7.4 The HN(C)N experiment EXERCISES APPENDIX A1. Hamiltonian of dipole-dipole interaction A2. Chemical Shift Anisotropy A3. Solid state NMR: basic features A4. Coherence selection by linear Field Gradients A5. Pure shift NMR: ZS and PSYCHE methods A6. HADAMARD NMR for selective excitation

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Book SynopsisThis textbook is designed for graduate students to introduce the basic concepts of Nuclear Magnetic Resonance spectroscopy (NMR), spectral analysis and modern developments such as multidimensional NMR, in reasonable detail and rigor. The book is self-contained, so, a unique textbook in that sense with end of chapter exercises included supported by a solution manual. Some of the advanced topics are included as Appendices for quick reference. Students of chemistry who have some exposure to mathematics and physics will benefit from this book and it will prepare them to pursue research in different branches of Chemistry or Biophysics or Structural Biology.​Table of ContentsChapter-1: BASIC CONCEPTS 1.1 Nuclear Spin and Magnetic Moments 1.2 Nuclear Spins in a Magnetic Field 1.3 Spin Lattice Relaxation 1.4 Spin temperature 1.5 Resonance Absorption of Energy and The NMR Experiment 1.5.1. The basic NMR spectrometer 1.6 Kinetics of Resonance Absorption 1.7 Selection Rules 1.8 Line widths 1.9 Bloch equations 1.10 More about relaxation 1.11 Sensitivity EXERCISES CHAPTER 2: HIGH RESOLUTION NMR SPECTRA OF MOLECULES 2.1 Introduction 2.2 Chemical Shift 2.2.1 Anisotropy of chemical shifts 2.2.2 Factors Influencing Isotropic Chemical shifts 2.3 Spin-Spin Coupling 2.4 Analysis of NMR spectra of molecules 2.4.1 First Order Analysis 2.4.2 Quantum Mechanical Analysis 2.5 Dynamic Effects in the NMR spectra 2.5.1 Two site Chemical Exchange 2.5.2. Collapse of spin multiplets 2.5.3 Conformational Averaging of J- values EXERCISES CHAPTER 3: FOURIER TRANSFORM NMR 3.1 Introduction 3.2 Principles of Fourier transform NMR 3.3 Theorems on Fourier transforms 3.4 The FTNMR Spectrometer 3.5. Practical aspects of recording FTNMR spectra 3.5.1. Carrier Frequency and off-set 3.5.2. RF pulse 3.5.3. Free Induction Decay (FID) and the spectrum 3.5.4. Single channel and quadrature detection 3.5.5. Signal digitization and sampling 3.5.6. Folding of signals 3.5.7. Acquisition time and the resolution 3.5.8. Signal averaging and Pulse repetition rate 3.6. Data processing in FT NMR 3.6.1. Zero filling 3.6.2. Digital filtration or window multiplication or apodization 3.7 Phase correction 3.8. Dynamic range in FTNMR 3.9. Spin-echo 3.10. Measurement of relaxation times 3.10.1. Measurement of relaxation time 3.10.2. Measurement of relaxation time 3.11. Water suppression through spin-echo: Watergate 3.12 Spin decoupling 3.13 Broad band decoupling 3.14 Biliniear Rotational Decoupling (BIRD) EXERCISES CHAPTER 4: POLARIZATION TRANSFER 4.1 Introduction 4.2 Experimental Schemes 4.3 Origin of NOE 4.3.1 A simplified treatment 4.3.2 A more rigorous treatment 4.4 Steady state NOE 4.5 Transient NOE 4.6. Selective population inversion 4.7. INEPT 4.7.1. Disadvantages of INEPT 4.8 Refocused INEPT 4.9 DEPT EXERCISES CHAPTER 5: Density matrix description of NMR 5.1 Introduction 5.2 Density matrix 5.3 Elements of Density Matrix 5.4. Time evolution of density operator 5.5. Matrix representations of RF pulses 5.6. Product Operator Formalism 5.6.1. Basis operator sets 5.6.2. Time-evolution of Cartesian Basis Operators 5.6.2.1 Free evolution under the influence of the Hamiltonian 5.6.2.2 Chemical Shift evolution 5.6.2.3 Scalar coupling evolution 5.6.2.4 Rotation by pulses 5.6.2.5 Calculation of the spectrum of J-coupled two spin system EXERCISES Chapter 6: Multidimensional NMR Spectroscopy 6.1 Segmentation of the time axis 6.2 Two dimensional NMR 6.3 Two-dimensional Fourier Transformation in NMR 6.4 Peak shapes in 2D spectrum 6.5 Quadrature detection in two-dimensional NMR 6.6 Types of 2D-NMR spectra 6.6.1 2D- resolution/ separation experiments 6.6.2. Two-dimensional correlation experiments 6.6.2.1 The COSY experiment 6.6.2.1.1 COSY of two-spins 6.6.2.1.2 COSY of three-spins 6.6.2.1.3 Disadvantages of COSY 6.6.2.2 Double-Quantum Filtered COSY (DQF-COSY) 6.6.2.3 Total Correlation Spectroscopy (TOCSY) 6.6.2.4 Two-dimensional Nuclear Overhauser Effect spectroscopy (2D-NOESY) 6.6.2.5 Two-dimensional ROESY 6.6.3 Two-dimensional heteronuclear correlation experiments 6.6.3.1 Heteronuclear COSY 6.6.3.2 Heteronuclear Multiple Bond Correlation (HMBC) 6.6.3.3 Combination of mixing sequences 6.7 Three dimensional NMR 6.7.1 The CT-HNCA experiment 6.7.2 The HNN experiment 6.7.3 The constant-time HN(CO)CA experiment 6.7.4 The HN(C)N experiment EXERCISES APPENDIX A1. Hamiltonian of dipole-dipole interaction A2. Chemical Shift Anisotropy A3. Solid state NMR: basic features A4. Coherence selection by linear Field Gradients A5. Pure shift NMR: ZS and PSYCHE methods A6. HADAMARD NMR for selective excitation

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Book SynopsisFrom complex structure elucidation to biomolecular interactions - this applicationoriented textbook covers both theory and practice of modern NMR applications. Part one sets the stage with a general description of NMR introducing important parameters such as the chemical shift and scalar or dipolar couplings. Part two describes the theory behind NMR, providing a profound understanding of the involved spin physics, deliberately kept shorter than in other NMR textbooks, and without a rigorous mathematical treatment of all the physico-chemical computations. Part three discusses technical and practical aspects of how to use NMR. Important phenomena such as relaxation, exchange, or the nuclear Overhauser effects and the methods of modern NMR spectroscopy including multidimensional experiments, solid state NMR, and the measurement of molecular interactions are the subject of part four. The final part explains the use of NMR for the structure determination of selected classes of complex biomolecules, from steroids to peptides or proteins, nucleic acids, and carbohydrates. For chemists as well as users of NMR technology in the biological sciences.Table of ContentsPreface INTRODUCTION TO NMR SPECTROSCOPY Our First 1D Spectrum Some Nomenclature: Chemical Shifts, Line Widths, and Scalar Couplings Interpretation of Spectra: A Simple Example Two-Dimensional NMR Spectroscopy: An Introduction PART ONE - Basics of Solution NMR BASICS OF 1D NMR SPECTROSCOPY The Principles of NMR Spectroscopy The Chemical Shift Scalar Couplings Relaxation and the Nuclear Overhauser Effect Practical Aspects Problems 1H NMR General Aspects Chemical Shifts Spin Systems, Symmetry, and Chemical or Magnetic Equivalence Scalar Coupling 1H-1H Coupling Constants Problems NMR OF 13C AND HETERONUCLEI Properties of Heteronuclei Indirect Detection of Spin-1/2 Nuclei 13C NMR Spectroscopy NMR of Other Main Group Elements NMR Experiments with Transition Metal Nuclei Problems PART TWO - Theory of NMR Spectroscopy NUCLEAR MAGNETISM - A MICROSCOPIC VIEW The Origin of Magnetism Spin - An Intrinsic Property of Many Particles Experimental Evidence for the Quantization of the Dipole Moment: The Stern-Gerlach Experiment The Nuclear Spin and Its Magnetic Dipole Moment Nuclear Dipole Moments in a Homogeneous Magnetic Field: The Zeeman Effect Problems MAGNETIZATION - A MACROSCOPIC VIEW The Macroscopic Magnetization Magnetization at Thermal Equilibrium Transverse Magnetization and Coherences Time Evolution of Magnetization The Rotating Frame of Reference RF Pulses Problems CHEMICAL SHIFT AND SCALAR AND DIPOLAR COUPLINGS Chemical Shielding The Spin-Spin Coupling Problems A FORMAL DESCRIPTION OF NMR EXPERIMENTS: THE PRODUCT OPERATOR FORMALISM Description of Events by Product Operators Classification of Spin Terms Used in the POF Coherence Transfer Steps An Example Calculation for a Simple 1D Experiment A BRIEF INTRODUCTION INTO THE QUANTUM-MECHANICAL CONCEPT OF NMR Wave Functions, Operators, and Probabilities Mathematical Tools in the Quantum Description of NMR The Spin Space of Single Noninteracting Spins Hamiltonian and Time Evolution Free Precession Representation of Spin Ensembles - The Density Matrix Formalism Spin Systems PART THREE - Technical Aspects of NMR THE COMPONENTS OF AN NMR SPECTROMETER The Magnet Shim Systems and Shimming The Electronics The Probehead The Lock System Problems ACQUISITION AND PROCESSING The Time Domain Signal Fourier Transform Technical Details of Data Acquisition Data Processing Problems EXPERIMENTAL TECHNIQUES RF Pulses Pulsed Field Gradients Phase Cycling Decoupling Isotropic Mixing Solvent Suppression Basic 1D Experiments Measuring Relaxation Times The INEPT Experiment The DEPT Experiment Problems THE ART OF PULSE EXPERIMENTS Introduction Our Toolbox: Pulses, Delays, and Pulsed Field Gradients The Excitation Block The Mixing Period Simple Homonuclear 2D Sequences Heteronuclear 2D Correlation Experiments Experiments for Measuring Relaxation Times Triple-Resonance NMR Experiments Experimental Details Problems PART FOUR - Important Phenomena and Methods in Modern NMR RELAXATION Introduction Relaxation: The Macroscopic Picture The Microscopic Picture: Relaxation Mechanisms Relaxation and Motion Measuring 15N Relaxation to Determine Protein Dynamics Measurement of Relaxation Dispersion Problems THE NUCLEAR OVERHAUSER EFFECT Introduction The Formal Description of the NOE: The Solomon Equations Applications of the NOE in Stereochemical Analysis Practical Tips for Measuring NOEs Problems CHEMICAL AND CONFORMATIONAL EXCHANGE Two-Site Exchange Experimental Determination of the Rate Constants Determination of the Activation Energy by Variable-Temperature NMR Experiments Problems TWO-DIMENSIONAL NMR SPECTROSCOPY Introduction The Appearance of 2D Spectra Two-Dimensional NMR Spectroscopy: How Does It Work? Types of 2D NMR Experiments Three-Dimensional NMR Spectroscopy Practical Aspects of Measuring 2D Spectra Problems SOLID-STATE NMR EXPERIMENTS Introduction The Chemical Shift in the Solid State Dipolar Couplings in the Solid State Removing CSA and Dipolar Couplings: Magic-Angle Spinning Reintroducing Dipolar Couplings under MAS Conditions Polarization Transfer in the Solid State: Cross-Polarization Technical Aspects of Solid-State NMR Experiments Problems DETECTION OF INTERMOLECULAR INTERACTIONS Introduction Chemical Shift Perturbation Methods Based on Changes in Transverse Relaxation (Ligand-Observe Methods) Methods Based on Changes in Cross-Relaxation (NOEs) (Ligand-Observe or Target-Observe Methods) Methods Based on Changes in Diffusion Rates (Ligand-Observe Methods) Comparison of Methods Problems PART FIVE - Structure Determination of Natural Products by NMR CARBOHYDRATES The Chemical Nature of Carbohydrates NMR Spectroscopy of Carbohydrates Quick Identification A Worked Example: Sucrose STEROIDS Introduction A Worked Example: Prednisone PEPTIDES AND PROTEINS Introduction The Structure of Peptides and Proteins NMR of Peptides and Proteins Assignment of Peptide and Protein Resonances A Worked Example: The Pentapeptide TP5 NUCLEIC ACIDS Introduction The Structure of DNA and RNA NMR of DNA and RNA Assignment of DNA and RNA Resonances APPENDIX The Magnetic H and B Fields Magnetic Dipole Moment and Magnetization Scalars, Vectors, and Tensors Properties of Matrices

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