Principles of High Resolution NMR in Solids


Book Description

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


Book Description

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.




High Resolution NMR Spectroscopy in Solids


Book Description

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.




High Resolution Solid-State NMR of Silicate and Zeolites


Book Description

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.




Modern Techniques in High-Resolution FT-NMR


Book Description

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.




Solid State NMR


Book Description

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.




Solid State NMR of Polymers


Book Description

In polymer science and technology, the advanced development of various new polymer materials with excellent properties and functions is desirable. For this purpose it is necesary to determine the exact relationship between physical properties and molecular structure-dynamics with powerful techniques. One such technique is solid state NMR. Recently, high resolution NMR studies of solids have been realized by using advanced pulse and mechanical techniques, which has resulted in a variety of structural and dynamical information on polymer systems. Solid state NMR has provided characteristic information which cannot be obtained by other spectroscopic methods.This book is divided into two parts. The first part covers the principles of NMR, important NMR parameters such as chemical shifts, relaxation times, dipolar interactions, quadrupolar interactions, pulse techniques and new NMR methods. In the second part, applications of NMR to a variety of polymer systems in the solid state are described.Features of this book:• Contains an up-to-date and comprehensive account of solid state NMR of polymers by leading researchers in the field• Provides a compilation of solid state NMR of polymers, which makes it an ideal reference book for both NMR researchers and general polymer scientists.This book will be of interest to the NMR community, and will be invaluable for both the beginner and the expert.




Modern Methods in Solid-state NMR


Book Description

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.




Solid-State NMR


Book Description

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.




NMR of Paramagnetic Molecules


Book Description

NMR of Paramagnetic Molecules: Principles and Applications is a compendium of papers that discusses the physical principles behind the technique of nuclear magnetic resonance, as well as, evaluates the scope and limitation of the applications of NMR in chemistry and biology. These papers emphasize the applications of the technique in chemistry and biochemistry where it widely used, particularlyon NMR experiments in the liquid state. Some papers describe the theoretical factors governing the resonance position and linewidth, and then also interpret magnetic resonance parameters in terms of electronic structure. Another paper investigates the gap between the mathematical complexities of earlier experiments and the operational aspects of chemical information from the spectra. Examples show studies in biochemical molecules and process in events where contact interactions are present either as a result of intrinsic molecular paramagnetism or are just induced through the addition of suitable paramagnetic probes. One paper presents the definitive and controversial results involving stereochemistry and deuterium NMR. This collection of papers will prove useful for nuclear physicists, researchers, and academicians in the field of nuclear physics.