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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.
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.
Covers the dramatic developments in the past decade in the applications of high-resolution NMR to the study of solid materials such as inorganic silicates, aluminosilicates, and in particular, zeolites. Also covers a variety of NMR methods, including conventional FT NMR techniques, used to investigate sorbate-sorbent interactions and the structure of adsorbed molecules. Gives an historical background to the subject and a concise survey of basic principles and methods of high-resolution solid-state NMR. Then covers 29Si NMR of silicate solutions; general aspects of 29Si and 27Al NMR of the silicate and aluminosilicate framework; application of 29Si and 27Al NMR to silicates, aluminosilicates, and zeolites; NMR studies of nuclei other than 29Si and 27Al in zeolites and non-zeolitic silicates; high-resolution studies of adsorbed molecules, and much more.
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.
This 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. This dual requirement is met through careful construction of the material within each chapter. The book is divided into two parts: "Fundamentals" and "Further Applications." The section on Fundamentals contains relatively long chapters that deal with the basic theory and practice of solid-state NMR. The essential differences and extra scope of solid-state NMR over solution-state is dealt with in an introductory chapter. The basic techniques that all chapters rely on are collected into a second chapter to avoid unnecessary repetition later. Remaining chapters in the "Fundamentals" part deal with the major areas of solid-state NMR which all solid-state NMR spectroscopists should know about. Each begins with an overview of the topic that puts the chapter in context. The basic principles upon which the techniques in the chapter rely are explained in a separate section. Each of these chapters exemplifies the principles and techniques with the applications most commonly found in current practice. The "Further Applications" section contains a series of shorter chapters which describe the NMR techniques used in other, more specific areas. The basic principles upon which these techniques rely will be expounded only if not already in the Fundamentals part.
NMR spectroscopy is the most valuable and versatile analytical tool in chemistry. While excellent monographs exist on high-resolution NMR in liquids and solids, this is the first book to address multidimensional solid-state NMR. Multidimensional techniques enable researchers to obtain detailed information about the structure, dynamics, orientation, and phase separation of solids, which provides the basis of a better understanding of materials properties on the molecular level.Dramatic progress-much of it pioneered by the authors-has been achieved in this area, especially in synthetic polymers. Solid-state NMR now favorably competes with well-established techniques, such as light, x-ray, or neutron scattering, electron microscopy, and dielectric and mechanical relaxation.The application of multidimensional solid-state NMR inevitably involves use of concepts from different fields of science. This book also provides the first comprehensive treatment of both the new experimental techniques and the theoretical concepts needed in more complex data analysis. The text addresses spectroscopists and polymer scientists by treating the subject on different levels; descriptive, technical, and mathematical approaches are used when appropriate. It presents an overview of new developments with numerous experimental examples and illustrations, which will appeal to readers interested in both the information content as well as the potential of solid-state NMR. The book also contains many previously unpublished details that will be appreciated by those who want to perform the experiments. The techniques described are applicable not only to the study of synthetic polymers but to numerous problems in solid-state physics, chemistry, materials science, and biophysics. - Presents original theories and new perspectives on scattering techniques - Provides a systematic treatment of the whole subject - Gives readers access to previously unpublished material - Includes extensive illustrations
Solid-state NMR covers an enormous range of material types and experimental techniques. Although the basic instrumentation and techniques of solids NMR are readily accessible, there can be significant barriers, even for existing experts, to exploring the bewildering array of more sophisticated techniques. In this unique volume, a range of experts in different areas of modern solid-state NMR explain about their area of expertise, emphasising the “practical aspects” of implementing different techniques, and illustrating what questions can and cannot be addressed. Later chapters address complex materials, showing how different NMR techniques discussed in earlier chapters can be brought together to characterise important materials types. The volume as a whole focusses on topics relevant to the developing field of “NMR crystallography” – the use of solids NMR as a complement to diffraction crystallography. This book is an ideal complement to existing introductory texts and reviews on solid-state NMR. New researchers wanting to understand new areas of solid-state NMR will find each chapter to be the equivalent to spending time in the laboratory of an internationally leading expert, learning the hints and tips that make the difference between knowing about a technique and being ready to put it into action. With no equivalent on the market, it will be of interest to every solid-state NMR researcher (academic and postgraduate) working in the chemical sciences.
The magnetism of nuclear spin systems has proved an amazingly fertile ground for the creativity of researchers. This happy circumstance results from the triple benediction that nature appears to have bestowed on nuclear spins: they are sporting spies-being infinitely manipulable (one is even tempted to say malleable), not unduly coy in revealing their secrets, and having a whole treasure house of secrets to reveal in the first place. researcher with Since spin dynamics are now orchestrated by the NMR ever more subtle scores, it is important to be able to tune into the pro ceedings with precision, if one is to make sense of it at all. Fortunately, it is not terribly difficult to do so, since in many ways spin dynamics are the theoretician's dream come true: they are often finite dimensional and quite tractable with basic quantum mechanics, frequently allowing near exact treatments and readily testable predictions. This book was conceived two years ago, with the objective of providing a simple, consistent introduction to the description of the spin dynamics that one encounters in modern NMR experiments. We believed it was a good time to attempt this, since it was possible by then to give sufficiently general descriptions of powelful classes of new NMR experiments. The choice of experiments we discuss in detail is necessarily subjective, al though we hope to have given a flavor of most of the important classes of pulse sequences, including some surface coil imaging applications.
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.