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Multinuclear Solid-State Nuclear Magnetic Resonance of Inorganic Materials

Author : Kenneth J.D. MacKenzie
Publisher : Elsevier
Page : 748 pages
File Size : 42,80 MB
Release : 2002-04-26
Category : Science
ISBN : 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 II

Author : Bernhard Blümich
Publisher : Springer
Page : 236 pages
File Size : 34,83 MB
Release : 1993-12-21
Category : Science
ISBN : 9783540571902

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1. G. Engelhardt, H. Koller, Stuttgart, FRG: 29Si NMR of Inorganic Solids 2. H. Pfeifer, Leizpig, FRG: NMR of Solid Surfaces 3. A. Sebald, Bayreuth, FRG: MAS and CP/MAS NMR of Less Common Spin-1/2 Nuclei 4. C. J{ger, Mainz, FRG: Satellite Transition Spectroscopy of Quadrupolar Nuclei 5. D. Brinkmann, M. Mali, Z}rich, CH: NMR-NQR Studies of High-Temperature Superconductors

Solid-state Nuclear Magnetic Resonance Spectroscopy of Unreceptive Quadrupolar Nuclei in Inorganic Materials

Author : Andre Sutrisno
Publisher :
Page : pages
File Size : 40,71 MB
Release : 2012
Category :
ISBN :

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Preparation and characterization of inorganic materials is a crucial practice because understanding the relationship between structure and property is important for improving current performance and developing novel materials. Many metal centers in technologically and industrially important materials are unreceptive low- quadrupolar nuclei (i.e., possessing low natural abundance, low NMR frequencies and large quadrupole moments) and they usually give rise to very broad NMR resonances and low signal-to-noise ratios, making it difficult to acquire their solid-state NMR spectra. This thesis focuses on the characterization of inorganic materials using solid-state NMR (SSNMR) spectroscopy at very high magnetic field of 21.1 T in combination with quantum chemical calculations for computational modeling. In the first part of this thesis, 67Zn and 17O SSNMR studies of several microporous materials were reported. The results of 67Zn SSNMR studies from several important metal-organic frameworks (MOFs), in particular, zeolitic imidazolate frameworks (ZIFs) were presented. 67Zn SSNMR spectroscopy was used to gain structural information regarding the desolvation process in MOF-5. Furthermore, 67Zn SSNMR spectroscopy were utilized to study the host-guest interactions in ZIF-8 loaded with different guest molecules. Static 67Zn SSNMR spectra of microporous zinc phosphites (ZnP) and zinc phosphates (ZnPO) were also acquired at natural abundance. The Gaussian calculation results on a model cluster for ZnP indicate that Zn-O bond length is the most dominant factor to the observed quadrupolar coupling constant (CQ) among other geometric parameters around Zn centres. The local structures of the framework oxygen sites in molecular sieve SAPO-34 were directly probed by several 17O SSNMR techniques. The involvement of water vapor during the SAPO-34 formation in dry-gel conversion (DGC) synthesis was also investigated. In the second part, 91Zr and 33S SSNMR spectra of layered zirconium phosphates (ZrP) and transition metal disulfides (MS2) were obtained. The empirical correlations between NMR parameters and various structural parameters were used for obtaining partial structural information in Li+ and Co(NH3)63+ exchanged layered ZrP. For a series of closely related MS2 materials, the observed differences in the CQ(33S) values were rationalized by considering the difference in their geometrical arrangements. The final part of this thesis featured two examples of SSNMR spectroscopy of exotic nuclei in some interesting inorganic materials. (i) The experimental 135/137Ba SSNMR spectroscopy and theoretical studies of -BBO, an important non-linear optical (NLO) material, indicate that the true crystal structure of -BBO is R3c space group rather than R3. (ii) An ultrahigh field natural abundance 73Ge SSNMR study of two representative germanium containing materials [GeCl2-dioxane and GePh4] demonstrated that acquiring 73Ge wideline NMR spectra of germanium compounds where the Ge experiences an extremely large quadrupolar interaction is feasible and that the small 73Ge chemical shielding anisotropy (CSA) can be directly measured.

Solid-State NMR III Organic Matter

Author : Bernhard Blümich
Publisher : Springer
Page : 232 pages
File Size : 35,80 MB
Release : 1994-11-04
Category : Science
ISBN : 9783540573999

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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 atNMR meetings, approaching that ofliquid state resonance. Important progress can be observed in three areas: Methodological developments, applications to inorganic matter, and applications to organic matter. These developments are intented to be captured in three volumes in this series, each of them being devoted to more or less one of these areas. The present volume on Solid-State NMR III is devoted mainly to organic matter. The recent developments of deuteron NMR and their applications are reviewed in the first chapter. Crosspolarization, MAS, and dynamic angle spinning are being explored for enhancement of information and sensitivity. In addition to the analysis of classical relaxation times and modern 2D spectra, detailed dynamic information becomes accessible from investigations of the relaxation time anisotropies. The second chapter examines cross-polarization in static and rotating solids under conditions of spin diffusion and thermal motion. The underlying dipole-dipole interaction is further exploited by the techniques described in the third chapter for studies of polymer-polymer miscibility. Short range techniques are discriminated from long-range techniques based on spin diffusion. The use ofthese techniques is illustrated by a case study ofPMMAJPVF blends. The last chapter addresses novel z methods and applications of two-dimensional exchange NMR for investigations of relative molecular orientations, polymer morphology, molecular dynamics, and macroscopic molecular order.