Solid-state nuclear magnetic resonance (SSNMR) is a powerful tool for the study of chemical structure and dynamics. The interactions that manifest in NMR spectra are anisotropic (id est, orientation dependent) in origin, often resulting in inhomogeneous broadening that can yield spectra exceeding circa 250 kHz in breadth; such spectra are often referred to as ultra-wideline (UW) NMR spectra. In many cases, UWNMR spectra cannot be acquired using conventional methods and rectangular radiofrequency (RF) pulses - rather, specialized pulses and techniques must be implemented. Furthermore, the large suite of high-resolution methods based on magic-angle spinning (MAS) are generally unsuitable for the acquisition of UWNMR spectra. Frequency-swept (FS) pulses are amplitude- and phase-modulated pulses that can irradiate NMR frequencies over large bandwidths. One of these is the wideband uniform-rate smooth-truncation (WURST) pulse, which features a linear effective frequency sweep. WURST pulses are used in the WURST-Carr-Purcell/Meiboom-Gill (WURST-CPMG) and broadband adiabatic inversion-cross polarization (BRAIN-CP) pulse sequences, which have been shown to be effective for the acquisition of UWNMR spectra of stationary (static) samples. These sequences have limitations, and to date, their capabilities have not been fully explored, nor have they been described from a theoretical point of view in a comprehensive manner.Signal processing is an integral component of pulsed-Fourier transform NMR spectroscopy, and comprises many protocols for enhancing spectral sensitivity and resolution. There has been much interest in advanced spectral processing methods such as alternate basis transformations (id est, besides Fourier encoding), statistical analyses (e.g., singular value decomposition, SVD, and principal component analysis, PCA), numerical regression (e.g., non-negative least squares), and the use of deep learning and neural networks. Such methodologies are now routinely implemented in imaging and multidimensional solution NMR, but are seldom explored in SSNMR. This thesis describes the development of new methods for the acquisition and advanced processing of conventional, wideline, and UW SSNMR spectra, including: (i) the design of new pulses and pulse sequences with optimal control theory (OCT); (ii) the modification of existing pulse sequences for UWNMR under MAS conditions; (iii) achieving signal enhancements with CPMG pulse sequences via the suppression of weak homonuclear dipolar coupling interactions under static and MAS conditions; (iv) the application of the BRAIN-CP pulse sequence to integer-spin nuclei, along with a thorough theoretical treatment; (v) rapid and robust measurements of longitudinal relaxation time constants (T1) and T1 anisotropies from UWNMR spectra under static conditions; (vi) the development and application of advanced processing methods for resolving UWNMR relaxation data with inverse Laplace transforms; and (vii) the development of a Python library for denoising 1D and 2D NMR spectra with SVD, PCA, and wavelet transforms. It is hoped that these methods will open up the Periodic Table of elements to increasingly routine exploration by SSNMR spectroscopy, aiding researchers in chemistry, biochemistry, materials science, and physics with advanced molecular-level characterization of their materials.

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 is a branch of Nuclear Magnetic Resonance which is presently experiencing a phase of strongly increasing popularity. The most striking evidence is the large number of contributions from Solid-State Resonance at NMR meetings, approaching that ofliquid state resonance. Important progress can be observed in the areas of methodological developments and applications to organic and inorganic matter. One volume devoted to more or less one of each of these areas has been published in the preceding three issues. This volume can be considered an addendum to this series. Selected methods and applications of Solid-State NMR are featured in three chapters. The first one treats the recoupling of dipolar interactions in solids, which are averaged by fast sample rotation. Following an introduction to effective Hamiltonians and Floquet theory, different types of experiment such as rotary resonance, dipolar chemical shift correlation spectroscopy, rotational resonance and multipulse recoupling are treated in the powerful Floquet formalism. In the second chapter, the different approaches to line narrowing of quadrupolar nuclei are reviewed in a. consistent formulation of double resonance (DaR) and dynamic angle spinning (DAS). Practical aspects of probe design are considered as well as advanced 2D experiments, sensitivity enhancement techniques, and spinning sideband manipulations. The use of such techniques dramatically increases the number of nuclei which can be probed in high resolution NMR spectroscopy. The final chapter describes new experimental approaches and results of structural studies of noncrystalline solids.

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.

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

Providing a definitive reference source on novel methods in NMR acquisition and processing, this book will highlight similarities and differences between emerging approaches and focus on identifying which methods are best suited for different applications. The highly qualified editors have conducted extensive research into the fundamentals of fast methods of data acquisition in NMR, including applications of non-Fourier methods of spectrum analysis. With contributions from additional distinguished experts in allied fields, clear explanations are provided on methods that speed up NMR experiments using different ways to manipulate the nuclei in the sample, modern methods for estimating the spectrum from the time domain response recorded during an NMR experiment, and finally how the data is sampled. Starting with a historical overview of Fourier Transformation and its role in modern NMR spectroscopy, this volume will clarify and demystify this important emerging field for spectroscopists and analytical chemists in industry and academia.