Principles of High Resolution NMR in Solids

Principles of High Resolution NMR in Solids

Author: M. Mehring

Publisher: Springer Science & Business Media

Published: 2012-12-06

Total Pages: 352

ISBN-13: 3642687563

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The field of Nuclear Magnetic Resonance (NMR) has developed at a fascinating pace during the last decade. It always has been an extremely valuable tool to the organic chemist by supplying molecular "finger print" spectra at the atomic level. Unfortunately the high resolution achievable in liquid solutions could not be obtained in solids and physicists and physical chemists had to live with unresolved lines open to a wealth of curve fitting procedures and a vast amount of speculations. High resolution NMR in solids seemed to be a paradoxon. Broad structure less lines are usually encountered when dealing with NMR in solids. Only with the recent advent of mUltiple pulse, magic angle, cross-polarization, two-dimen sional and multiple-quantum spectroscopy and other techniques during the last decade it became possible to resolve finer details of nuclear spin interactions in solids. I have felt that graduate students, researchers and others beginning to get involved with these techniques needed a book which treats the principles, theo retical foundations and applications of these rather sophisticated experimental techniques. Therefore I wrote a monograph on the subject in 1976. Very soon new ideas led to the developement of "two-dimensional spectroscopy" and "multiple-quantum spectroscopy", topics which were not covered in the first edition of my book. Moreover an exponential growth of literature appeared in this area of research leaving the beginner in an awkward situation of tracing back from a current article to the roots of the experiment.


High Resolution NMR in Solids Selective Averaging

High Resolution NMR in Solids Selective Averaging

Author: Ulrich Haeberlen

Publisher: Elsevier

Published: 2012-12-02

Total Pages: 205

ISBN-13: 0323160255

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High Resolution NMR in Solids: Selective Averaging presents the principles and applications of the four approaches to high resolution NMR in solids — magic-angle sample spinning, multiple-pulse, proton-enhanced nuclear induction, and indirect detection methods. Divided into six chapters, this book initially describes the tensorial properties of nuclear spin interactions in both ordinary and spin spaces. It then deals with the manifestations of nuclear magnetic shielding in NMR spectra of both single-crystal and powder samples, and then discusses the techniques for analyzing spectra and rotation patterns in terms of shielding tensors. A wide range of NMR phenomena that are result of intentional or natural, selective or unselective averaging processes and the average Hamiltonian theory that yields the inclusion of correction are covered. This book also provides a detailed discussion on multiple-pulse sequences intended for high resolution NMR in solids. The concluding chapter examines the applications of multiple-pulse techniques, with particular emphasis on measurements of 19F and 1H shielding tensors. Discussions on rotations of angular momentum operators; time ordering and the Magnus expansion; off-resonance averaging of the second-order dipolar Hamiltonian; and phase transients are covered in the supplemental texts.


Solid State NMR

Solid State NMR

Author: Klaus Müller

Publisher: John Wiley & Sons

Published: 2021-08-23

Total Pages: 562

ISBN-13: 352731816X

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Solid State NMR A thorough and comprehensive textbook covering the theoretical background, experimental approaches, and major applications of solid-state NMR spectroscopy Nuclear Magnetic Resonance (NMR) spectroscopy is a powerful non-destructive technique capable of providing information about the molecular structure and dynamics of molecules. Alongside solution-state NMR, a well-established technique to study chemical structures and investigate physico-chemical properties of molecules in solutions, solid-state NMR (SSNMR) offers many exciting possibilities for the analysis of solid and soft materials across scientific fields. SSNMR shows unique capabilities for a detailed investigation of structural and dynamic properties of materials over wide space and time ranges. For this reason, and thanks to significant advances in the past several years, the application of SSNMR to materials is rapidly increasing in disciplines such as chemistry, physics, and materials and life sciences. Solid State NMR: Principles, Methods, and Applications offers a systematic introduction to the theory, methodological concepts, and major experimental methods of SSMR spectroscopy. Exploring the unique potential of SSNMR for the structural and dynamic characterization of soft and either amorphous or crystalline solid materials, this comprehensive textbook provides foundational knowledge and recent developments of SSNMR, covering physical and theoretical background, experimental methods, and applications to pharmaceuticals, polymers, inorganic and hybrid materials, liquid crystals, and model membranes. Written by two expert authors to ensure a clear and consistent presentation of the subject, this textbook: Includes a brief introduction to the historical aspects and broad theoretical background of solid-state NMR spectroscopy Provides helpful illustrations to explain the various SSNMR concepts and methods Features accessible descriptive text with self-consistent use of quantum mechanics Covers the experimental aspects of SSNMR spectroscopy and in particular a description of many useful pulse sequences Contains references to relevant literature Solid State NMR: Principles, Methods, and Applications is the ideal textbook for university courses on SSNMR, advanced spectroscopies, and a valuable single-volume reference for spectroscopists, chemists, and researchers in the field of materials.


High Resolution NMR Spectroscopy in Solids

High Resolution NMR Spectroscopy in Solids

Author: M. Mehring

Publisher: Springer Science & Business Media

Published: 2012-12-06

Total Pages: 257

ISBN-13: 3642963323

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Manipulation and Dilution Tools for Ruling Abundant Species "NMR is dead" was the slogan heard in the late 1960s at least among physicists, until John S. Waugh and his co-workers initiated a series of new NMR experiments, which employed the coherent modulation of interactions by strong radiofrequency fields. A wealth of new phenomena was observed, which are summarized in the introduction for the convenience of the unbiased reader, whereas Section 2 collects the basic spin interactions observed in solids. Line-narrowing effects in dipolar coupled solids by the application of multiple pulse experiments are extensively discussed in Section 3. Numerous extensions of the basic Waugh, Huber, and Haeberlen experiment have been developed by different groups and have been applied to the nuclei IH, 9Be, 19F, 27Al, 31p, 63CU in solids. Application of this technique to a variety of systems is still in progress and should reveal interesting insights into weak spin interactions in solids. It was soon realized that rare spins could be used as monitors for molecular fields in the solid state; however, rare spin observation is difficult because of the small signal-to-noise ratio. Pines, Gibby, and Waugh introduced a new concept of cross-polarization, based on ideas of Hahn and co-workers, which allows the detection ofrare spins with increased sensitivity. The dynamics involved are treated in detail. Other sections merely list results obtained by the techniques described and demonstrate their usefulness in the investigation of dynamical problems in molec ular and solid state physics.


Multinuclear Solid-State Nuclear Magnetic Resonance of Inorganic Materials

Multinuclear Solid-State Nuclear Magnetic Resonance of Inorganic Materials

Author: Kenneth J.D. MacKenzie

Publisher: Elsevier

Published: 2002-04-26

Total Pages: 748

ISBN-13: 0080537103

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Techniques of solid state nuclear magnetic resonance (NMR) spectroscopy are constantly being extended to a more diverse range of materials, pressing into service an ever-expanding range of nuclides including some previously considered too intractable to provide usable results. At the same time, new developments in both hardware and software are being introduced and refined. This book covers the most important of these new developments. With sections addressed to non-specialist researchers (providing accessible answers to the most common questions about the theory and practice of NMR asked by novices) as well as a more specialised and up-to-date treatment of the most important areas of inorganic materials research to which NMR has application, this book should be useful to NMR users whatever their level of expertise and whatever inorganic materials they wish to study.


Solid-State NMR

Solid-State NMR

Author: David C. Apperley

Publisher: Momentum Press

Published: 2012-06-10

Total Pages: 280

ISBN-13: 1606503529

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The power of nuclear magnetic resonance, NMR, for characterizing molecules dissolved in solution is widely acknowledged and NMR forms an essential component of undergraduate chemistry degrees. However, the application of NMR to the solid state is much less well appreciated. This text sets out the fundamental principles of solid-state NMR, explaining how NMR in solids differs from that in solution, showing how the various interactions of NMR can be manipulated to yield high-resolution spectra and to give information on local structure and dynamics in solids. This book aims to take some of the mystique out of solid-state NMR by providing a comprehensible discussion of the methodology, including the basic concepts and a practical guide to implementation of the experiments. A basic knowledge of solution-state NMR is assumed and is only briefly covered. The text is intended for those in academia and industry expecting to use solid-state NMR in their research and looking for an accessible introduction to the field. It will also be valuable for non-experts interested in learning how NMR can be usefully applied to solid systems. Detailed mathematical treatments are delayed to a chapter at the mid-point of the text and can be skipped. Introductions to experiments and numerical simulations are provided to help link NMR results to experimental practice. The different aspects of solid-state NMR, from basic pulse-and-acquire experiments to sophisticated techniques for the measurement of anisotropy information are presented. Examples illustrate the wide variety of applications of the technique and its complementarity to other solid-state characterization techniques such as X-ray diffraction. Various aspects of NMR crystallography are covered as are topics of motion in solids.


Transient Techniques in NMR of Solids

Transient Techniques in NMR of Solids

Author: Bernard C. Gerstein

Publisher:

Published: 1985

Total Pages: 320

ISBN-13:

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This volume is an ideal starting point for the graduate student seeking a basic introduction to the theory and uses of solid-state nuclear magnetic resonance (NMR) spectroscopy. Accessible to students with only a survey-level physics background, the material assumes little prior knowledge of the basic theory of electromagnetism. All the major areas are covered, including an introduction to concepts of time-dependent quantum mechanics as they apply to NMR spectroscopy of the solid state. Each chapter includes problems designed to enhance the reader's understanding of the material. Instructive and practical, this volume provides the basic knowledge needed to access the general literature and the more advanced monographs on this subject. In addition to assisting entrance into the field, Transient Techniques in NMR of Solids will be a useful guide for professionals already working in related areas of chemistry. FROM THE PREFACE: Nuclear magnetic resonance (NMR) is truly a remarkable phenomenon. Remarkable can imply different things to different people. From the point of view of a physicist, spin dynamics is an elegant example of the use of time-dependent quantum mechanics, and NMR absorption of energy is a prototype for spectroscopic transitions. From the point of view of the practicing chemist and materials scientist, NMR spectroscopy is an invaluable tool for the identification of chemical species and structures. Had NMR spectroscopic techniques commercially available in the early 1960s been the only result of investigations of this phenomenon, it would have had a major impact on the course of chemical analysis. The study of liquids and solutions for chemical shifts and couplings of protons had produced a rapid means of identifying chemical species nondestructively. The study of dynamical properties also could be addressed by study of temperature dependence of the spectra or of the saturation of the resonance by high-power irradiation. Even at that time, however, studies of the spin dynamics had already begun to indicate that there were many interesting facets of the NMR phenomenon left to exploit. For example, the Fourier-transform relationship of the free-induction decay and the absorption spectrum had been shown and the basis of the cross-polarization experiment was being investigated. A number of chemists had begun to study the spin*b1lattice relaxation times of species by pulse NMR techniques by utilizing methods that were not familiar at that time to the typical chemist but that are now commonly employed in NMR analysis. The principal characteristic of the NMR technique that makes it so useful for chemical analysis of liquids and solutions is the high resolution that allows one to observe very small interactions such as the chemical shift and the spin*b1spin coupling. These weak interactions are quite sensitive to the local environment of the spin and therefore may be used as a diagnostic for the environment. The connectivity of chemical structure is often mimicked closely in the NMR connectivity of the spectrum, and quantitative informaton is relatively easy to obtain. Nuclear magnetic resonance spectra of solids exhibit such resolution only in special cases. The primary (although not the exclusive) reason for the lack of resolution in the spectrum of a typical solid is the presence of the dipole*b1dipole interaction, which dominates the NMR spectroscopy of solids that have been of interest to chemists. One solution (no pun intended) to the problem of obtaining chemical-shift information about such solids is to dissolve them and to study them in solution. However, if the solid is insoluble or otherwise intractable or if the analysis involves questions about the properties of the substance in the solid state, then there arises a need for techniques to study the weaker interactions in the presence of the dipole*b1dipole interaction or other overwhelming interactions. This volume describes the means dev


Nuclear Magnetic Resonance Spectroscopy

Nuclear Magnetic Resonance Spectroscopy

Author: Frank Alden Bovey

Publisher:

Published: 1969

Total Pages: 420

ISBN-13:

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Nine chapters cover: fundamental principles; experimental methods; the chemical shift; coupling of nuclear spins; nuclear relaxation and chemical rate processes; two-dimensional nuclear magnetic resonance spectroscopy; macromolecules; NMR of solids; special topics. Annotation copyrighted by Book News, Inc., Portland, OR


Nuclear Magnetic Resonance Spectroscopy

Nuclear Magnetic Resonance Spectroscopy

Author: Joseph B. Lambert

Publisher: John Wiley & Sons

Published: 2019-01-04

Total Pages: 485

ISBN-13: 1119295238

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Combines 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 that allows identification and characterization of organic, and some inorganic, compounds. It offers chapters covering: Experimental Methods; The Chemical Shift; The Coupling Constant; Further Topics in One-Dimensional NMR Spectroscopy; Two-Dimensional NMR Spectroscopy; Advanced Experimental Methods; and Structural Elucidation. Features classical analysis of chemical shifts and coupling constants for both protons and other nuclei, as well as modern multi‐pulse and multi-dimensional methods Contains experimental procedures and practical advice relative to the execution of NMR experiments Includes a chapter-long, worked-out problem that illustrates the application of nearly all current methods Offers appendices containing the theoretical basis of NMR, including the most modern approach that uses product operators and coherence-level diagrams By offering a balance between volumes aimed at NMR specialists and the structure-determination-only books that focus on synthetic organic chemists, Nuclear Magnetic Resonance Spectroscopy: An Introduction to Principles, Applications, and Experimental Methods, 2nd Edition is an excellent text for students and post-graduate students working in analytical and bio-sciences, as well as scientists who use NMR spectroscopy as a primary tool in their work.