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Book Local Structural Characterisation

Download or read book Local Structural Characterisation written by Duncan W. Bruce and published by John Wiley & Sons. This book was released on 2013-07-31 with total page 298 pages. Available in PDF, EPUB and Kindle. Book excerpt: Inorganic materials are at the heart of many contemporary real-world applications, in electronic devices, drug delivery, bio-inspired materials and energy storage and transport. In order to underpin novel synthesis strategies both to facilitate these applications and to encourage new ones, a thorough review of current and emerging techniques for materials characterisation is needed. Examining important techniques that allow investigation of the structures of inorganic materials on the local atomic scale, Local Structural Characterisation discusses: Solid-State NMR Spectroscopy X-Ray Absorption and Emission Spectroscopy Neutrons and Neutron Spectroscopy EPR Spectroscopy of Inorganic Materials Analysis of Functional Materials by X-Ray Photoelectron Spectroscopy This addition to the Inorganic Materials Series provides a detailed and thorough review of these spectroscopic techniques and emphasises the interplay between chemical synthesis and physical characterisation.

Book Solid state NMR Characterization of Polymeric and Inorganic Materials

Download or read book Solid state NMR Characterization of Polymeric and Inorganic Materials written by Jessi A. Baughman and published by . This book was released on 2015 with total page 173 pages. Available in PDF, EPUB and Kindle. Book excerpt: Multiple systems were studied to advance the understanding of the chemical composition of the materials. These materials contained various structures or structures within different physical phases. Solid-state NMR techniques were used to probe effects of different chemical processes and environmental conditions on the chemical structures and phase composition of these materials. Much of the high thermal and chemical resistance of poly(vinylidene-cohexafluoropropylene) is gained from cross-linking. The insolubility of the cross-linked fluoroelastomer has prevented the characterization of the structure at the cross-link site by NMR. Samples from each of the four stages of the cross-linking of poly(vinylideneco-hexafluoropropylene) were analyzed with solid-state NMR to determine the chemical structure at the cross-linking site and the effects of cross-linking on the mobility of the elastomer chains. Spectral overlap from chemical shift dispersion hindered the use of simple 1D techniques to assign structural components to peaks in the NMR spectra. Relaxation studies that measured T1, T2, and T1[subscript p] relaxation times were used to assign new peaks in the NMR spectra to the fluoride salts that are produced during cross-linking. The NMR relaxation data also indicated no reduction in the mobility of the fluoroelastomer from cross-linking. The chemical structure of the cross-link site was partially characterized by 2D-NMR. However, the amorphous nature of the polymer inhibited a full characterization of this location with 2D-NMR techniques. The structures that were identified at the cross-link site supported proposed structures. Solutions of NaCl and dextrose used in the preservation of premixed drugs were analyzed to distinguish the solid and liquid phases over a temperature range of -60 to 20 °C. The large chemical shift dispersion in the NMR spectra made analysis of the frequency domain data difficult. The time domain data of the single pulse NMR experiments were analyzed using a logarithmic fitting technique and the inverse LaPlace transform. The logarithmic fit technique was able to distinguish a single solid and a single liquid phase for the NaCl and dextrose solutions. The inverse LaPlace transform indicated the presence of three phases near the center of the temperature range. The additional phase was assigned to a liquid phase of concentrated solution based on the T2 time of the phase found by the inverse LaPlace transform. The two methods gave similar results and were used to identify the percentage of each phase present throughout the temperature range. 33S solid-state NMR was used to characterize the discharge products of a lithium-sulfur battery. A single pulse experiment with a solid echo was used to help minimize the broadening effects of the quadrupolar interactions in 33S. Li2S was detected in the cathode of the fully discharged battery. Longer lithium sulfide polymer chains expected at higher discharge potentials were not detected due to large line widths in the NMR spectrum and small sample size that severely reduced the signal-to-noise. A reduced signal-to-noise spectrum of natural abundance, elemental sulfur suggested an isotropic chemical shift at -50 ppm.

Book Solid State NMR

    Book Details:
  • Author : Klaus Müller
  • Publisher : John Wiley & Sons
  • Release : 2021-06-23
  • ISBN : 3527690115
  • Pages : 560 pages

Download or read book Solid State NMR written by Klaus Müller and published by John Wiley & Sons. This book was released on 2021-06-23 with total page 560 pages. Available in PDF, EPUB and Kindle. Book excerpt: 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.

Book Solid state NMR as a Powerful Tool to Characterize Polysaccharide based Systems

Download or read book Solid state NMR as a Powerful Tool to Characterize Polysaccharide based Systems written by Francesco D'Acierno and published by . This book was released on 2017 with total page pages. Available in PDF, EPUB and Kindle. Book excerpt: An accurate structural characterization of polysaccharide-based systems is crucial in understanding the properties of the materials. Among all the characterization techniques, solid-state NMR spectroscopy proves to be fundamental for a clear picture of complex polysaccharide-based systems. An example of complexity in these systems is represented by disordered structures. Polysaccharides with large fractions of amorphous regions can be analyzed using 1H-13C cross-polarization (CP) magic-angle-spinning (MAS) to resolve their molecular sites. The same experiment can be applied to biochars obtained by thermal degradation of biopolymers to quantitatively characterize the forms of carbon present, in combination with direct polarization (DP) MAS to determine the size of the carbonaceous char clusters. Solid-state NMR is also effective in the structural characterization of porous materials. Some polysaccharides, such as chitin, self-assemble in mesoporous architectures directly in nature, while for others, such as cellulose, reduction to a nanocrystalline form is required to obtain these types of networks. Mesoporous polysaccharide-based materials can often be used as templates to create inorganic materials with complementary porosity, such as alumina aerogels, which can be exploited as catalyst supports, absorbents, or thermal insulators. Solid-state NMR enables the structural characterization of the biotemplated materials, when the corresponding isotope is NMR-sensitive. In this presentation, I will discuss our use of solid-state NMR techniques to probe the structures of new materials developed from biopolymers. This technique gives insight into the structure of the materials that is not available from other analytical methods.

Book Heteronuclear X Y Double Resonance Solid State NMR

Download or read book Heteronuclear X Y Double Resonance Solid State NMR written by Christopher John Hudalla and published by . This book was released on 1997 with total page 163 pages. Available in PDF, EPUB and Kindle. Book excerpt:

Book Solid state NMR Spectroscopy of Inorganic Materials

Download or read book Solid state NMR Spectroscopy of Inorganic Materials written by John J. Fitzgerald and published by . This book was released on 1999 with total page 440 pages. Available in PDF, EPUB and Kindle. Book excerpt: This book strikes a balance between state-of-the-art solid-state NMR techniques and the applications of these techniques to problems in materials science. The applications focus on modern inorganic materials such as metal oxides, catalysts, zeolites, glasses, ceramics, semiconductors, ion conductors, superconductors, and composites. The book features chapters on multiple-quantum MAS NMR, dynamic-angle spinning NMR for quadrupolar nuclides, and two-dimensional NMR methods. It includes an introductory chapter that provides an a thorough and integrated overview of the field, complete with numerous references.

Book Solid State NMR in Zeolite Catalysis

Download or read book Solid State NMR in Zeolite Catalysis written by Jun Xu and published by Springer. This book was released on 2019-05-11 with total page 260 pages. Available in PDF, EPUB and Kindle. Book excerpt: Solid-State NMR Characterization of Heterogeneous Catalysts and Catalytic Reactions provides a comprehensive account of state-of-the-art solid-state NMR techniques and the application of these techniques in heterogeneous catalysts and related catalytic reactions. It includes an introduction to the basic theory of solid-state NMR and various frequently used techniques. Special emphasis is placed on characterizing the framework and pore structure, active site, guest-host interaction, and synthesis mechanisms of heterogeneous catalysts using multinuclear one- and two-dimensional solid-sate NMR spectroscopy. Additionally, various in-situ solid-state NMR techniques and their applications in investigation of the mechanism of industrially important catalytic reactions are also discussed. Both the fundamentals and the latest research results are covered, making the book suitable as a reference guide for both experienced researchers in and newcomers to this field. Feng Deng is a Professor at Wuhan Institute of Physics and Mathematics, Chinese Academy of Sciences.

Book NMR Methods for Characterization of Synthetic and Natural Polymers

Download or read book NMR Methods for Characterization of Synthetic and Natural Polymers written by Rongchun Zhang and published by Royal Society of Chemistry. This book was released on 2019-07-29 with total page 590 pages. Available in PDF, EPUB and Kindle. Book excerpt: Since the introduction of FT-NMR spectroscopy around five decades ago, NMR has achieved significant advances in hardware and methodologies, accompanied with the enhancement of spectral resolution and signal sensitivity. Rapid developments in the polymers field mean that accurate and quantitative characterization of polymer structures and dynamics is the keystone for precisely regulating and controlling the physical and chemical properties of the polymer. This book specifically focuses on NMR investigation of complex polymers for the polymer community as well as NMR spectroscopists, and will push the development of both fields. It covers the latest advances, for example high field DNP and ultrafast MAS methodologies, and show how these novel NMR methods characterize various synthetic and natural polymers.

Book Frustrated Lewis Pairs I

Download or read book Frustrated Lewis Pairs I written by Gerhard Erker and published by Springer. This book was released on 2014-07-08 with total page 354 pages. Available in PDF, EPUB and Kindle. Book excerpt: Discovery of Frustrated Lewis Pairs: Intermolecular FLPs for Activation of Small Molecules, by Douglas W. Stephan Intramolecular Frustrated Lewis Pairs: Formation and Chemical Features, by Gerald Kehr, Sina Schwendemann, Gerhard Erker Frustrated Lewis Pair Mediated Hydrogenations, by Douglas W. Stephan, Gerhard Erker Amine-Borane Mediated Metal-Free Hydrogen Activation and Catalytic Hydrogenation, by Victor Sumerin, Konstantin Chernichenko, Felix Schulz, Markku Leskelä, Bernhard Rieger, Timo Repo Hydrogen Activation by Frustrated Lewis Pairs: Insights from Computational Studies, by Tibor András Rokob, Imre Pápai Quantum Chemistry of FLPs and Their Activation of Small Molecules: Methodological Aspects, by Birgitta Schirmer, Stefan Grimme Computational Design of Metal-Free Molecules for Activation of Small Molecules, Hydrogenation, and Hydroamination, by Zhi-Xiang Wang, Lili Zhao, Gang Lu, Haixia Li, Fang Huang Computational Studies of Lewis Acidity and Basicity in Frustrated Lewis Pairs, by Thomas M. Gilbert Solid-State NMR as a Spectroscopic Tool for Characterizing Phosphane - Borane Frustrated Lewis Pairs, by Thomas Wiegand, Hellmut Eckert, Stefan Grimme

Book Structural Characterization Techniques

Download or read book Structural Characterization Techniques written by Lorenzo Malavasi and published by CRC Press. This book was released on 2016-10-14 with total page 356 pages. Available in PDF, EPUB and Kindle. Book excerpt: This book presents state-of-the-art contributions related to advanced structural characterization techniques in the field of clean energy materials with particular emphasis on solid oxide fuel cells and hydrogen storage materials. It describes several diffraction and spectroscopic techniques for the investigation of both average and local structures with several examples of the most recent materials for clean energy applications. It is the first authoritative collection of contributions on the importance of the application of the most advanced structural techniques to shed light on the properties and mechanisms of materials currently investigated for the use in alternative energy devices. The book provides key techniques for ex situ and in situ investigation of clean energy materials and, hence, is an essential guide for researchers working on the structural analysis of advanced materials.

Book Structural Insights Into Group 14 Compounds from Solid State NMR Spectroscopy

Download or read book Structural Insights Into Group 14 Compounds from Solid State NMR Spectroscopy written by M. A. Hanson and published by . This book was released on 2012 with total page 402 pages. Available in PDF, EPUB and Kindle. Book excerpt: In this thesis, the potential utility of solid-state NMR spectroscopy to provide insights into the structure and bonding of organogermanium and tin compounds is examined. Germanium-73 is an extremely challenging nucleus to examine due to multiple unfavourable NMR properties. However, the great utility of silicon-29 NMR spectroscopy suggests that 73Ge could be a valuable tool for structural characterization. Initial investigations focused on a series of simple organogermanes as benchmarks for future investigations. Compounds with known X-ray structures were used to determine an effective method for density functional theory calculations. That methodology was then further employed to propose structures for several less well characterized compounds. 73Ge NMR spectroscopy was used, in conjunction with 35Cl and 79Br NMR spectroscopy, to characterize the novel germanium(I) halides, GeCl and GeBr. As the monohalides are amorphous, glasslike compounds, methods for structural characterization are limited. Calculation of the NMR parameters for a series of model compounds was used to propose a structure. 35Cl NMR spectroscopy was explored as a potential source of indirect information about germanium. There appears to be a relationship between the oxidation state at germanium and the shape of the 35Cl NMR signal. Additionally, a correlation between the NMR parameters of germanium(II) chlorides and Ge-Cl bond lengths was established. 119Sn NMR spectroscopy is better developed than 73Ge or 35Cl NMR spectroscopy. However, it is often difficult to obtain a 119Sn signal in solution at moderate magnetic iv fields. A series of cationic tin(II) cryptand complexes were examined in the solid state. The 119Sn NMR parameters were used to describe the structure of a compound for which X-ray quality single crystals could not be grown. Additionally, several ambiguities about the bonding of a second compound were resolved.

Book Solid State Chemistry of Inorganic Materials V  Volume 848

Download or read book Solid State Chemistry of Inorganic Materials V Volume 848 written by Materials Research Society. Meeting and published by . This book was released on 2005-07-18 with total page 568 pages. Available in PDF, EPUB and Kindle. Book excerpt: Solid-state chemistry continues to span and to spawn multiple materials research areas, attracting investigators from chemistry, condensed-matter physics, materials science and engineering, ceramics, chemical engineering, and mineralogy/geology, to name a few. The common challenge is to understand and to predict structures and properties of new materials. As with earlier volumes in this series from the Materials Research Society, the presentations here represent interdisciplinary research from around the world and explore not only recent advances in the solid-state chemistry of inorganic materials, but also their impact on commercial applications. The book covers a broad range of topics, including synthesis and characterization of novel functional materials; design and fabrication of nanostructures and nanomaterials; crystal and structural chemistry; catalysis; gas separation and storage; and magnetic and optical applications. Both theoretical and computational studies of solid-state inorganic materials are featured. Joint presentations with solid-state ionics are also particularly fruitful.

Book Structural Characterization of Noncrystalline Solids and Glasses Using Solid State NMR

Download or read book Structural Characterization of Noncrystalline Solids and Glasses Using Solid State NMR written by Hellmut Eckert and published by . This book was released on 1992 with total page 135 pages. Available in PDF, EPUB and Kindle. Book excerpt:

Book Handbook of Materials Characterization

Download or read book Handbook of Materials Characterization written by Surender Kumar Sharma and published by Springer. This book was released on 2018-09-18 with total page 612 pages. Available in PDF, EPUB and Kindle. Book excerpt: This book focuses on the widely used experimental techniques available for the structural, morphological, and spectroscopic characterization of materials. Recent developments in a wide range of experimental techniques and their application to the quantification of materials properties are an essential side of this book. Moreover, it provides concise but thorough coverage of the practical and theoretical aspects of the analytical techniques used to characterize a wide variety of functional nanomaterials. The book provides an overview of widely used characterization techniques for a broad audience: from beginners and graduate students, to advanced specialists in both academia and industry.