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Applied Medical Informatics     Open Access   (Followers: 10)
Arab Journal of Nephrology and Transplantation     Open Access   (Followers: 1)
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ARS Medica Tomitana     Open Access   (Followers: 1)
Art Therapy: Journal of the American Art Therapy Association     Full-text available via subscription   (Followers: 11)
Arterial Hypertension     Open Access   (Followers: 1)
Artificial Intelligence in Medicine     Hybrid Journal   (Followers: 12)
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ASHA Leader     Open Access  
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Asia Pacific Journal of Clinical Trials : Nervous System Diseases     Open Access  
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Asian Journal of Cell Biology     Open Access   (Followers: 5)
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ASPIRATOR : Journal of Vector-borne Disease Studies     Open Access  
Astrocyte     Open Access  
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Atti della Accademia Peloritana dei Pericolanti - Classe di Scienze Medico-Biologiche     Open Access  
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Journal Cover Annual Reports on NMR Spectroscopy
  [SJR: 0.627]   [H-I: 31]   [4 followers]  Follow
   Full-text available via subscription Subscription journal
   ISSN (Print) 0066-4103
   Published by Elsevier Homepage  [3162 journals]
  • Chapter One Accurate NMR Determinations of Proton–Proton Distances
    • Authors: Sándor Boros; Zoltán Gáspári; Gyula Batta
      Pages: 1 - 39
      Abstract: Publication date: 2018
      Source:Annual Reports on NMR Spectroscopy, Volume 94
      Author(s): Sándor Boros, Zoltán Gáspári, Gyula Batta
      There are obvious reasons why precise internuclear distance measurements are essential in structural chemistry. Here we wish to give a practice-oriented review on the topic of accurate proton–proton distance measurements by solution NMR. The history of NOE and ROE methods is quite long, and the ambition has always been to tackle with the distance problem in a quantitative sense. The reader can find a basic introduction to relaxation and incoherent magnetization transfer by cross-relaxation. With the improvement of NMR instrument technology and improved measuring pulse sequences it has become everyday practice to run NOE/ROE experiments. Though the principles of quantitative NOE experiments have been known for decades, the full potential of the methods is rarely used for either small or big molecules. Here we suggest those improved experimental methods and their evaluation protocols that can be followed for accurate distance determination. Improvements in NOESY and ROESY sequences are presented, as well as the possibility of the “exact NOE” option for biopolymers. Hopefully, the interested reader can apply the techniques explained in this review.

      PubDate: 2018-02-25T17:58:07Z
      DOI: 10.1016/bs.arnmr.2017.12.002
      Issue No: Vol. 94 (2018)
  • Chapter Two Recent Solid-State NMR Studies of Hydrated Lipid Membranes
    • Authors: Yuichi Umegawa; Nobuaki Matsumori; Michio Murata
      Pages: 41 - 72
      Abstract: Publication date: 2018
      Source:Annual Reports on NMR Spectroscopy, Volume 94
      Author(s): Yuichi Umegawa, Nobuaki Matsumori, Michio Murata
      Interactional and structural analyses of lipids in hydrated biomembranes are at the frontier of membrane physics and biology. Recently, solid-state NMR has emerged as a frequently used technique for the investigation of biomembrane systems, leading to particularly remarkable advances in the study of the structural biology of membrane proteins. However, conformational and interactional analyses of lipid molecules and membrane-active small compounds remain challenging. This chapter highlights recent applications of solid-state NMR to membrane lipids and nonpeptidic molecules such as membrane-active natural products. Lipid rafts are microdomains in cellular membranes formed by sphingomyelin and cholesterol and are thought to constitute a platform for signal transduction. Amphotericin B, theonellamide-A, and amphidinol 3 exert their activities by interacting with lipid membranes. Deuterium quadrupole coupling combined with dipole–dipole interactions has been used to evaluate the interaction modes and dynamic properties of membrane lipids and small membrane-active compounds. Herein, we review the recent advances in these topics using our recent research studies as examples of solid-state NMR investigations of hydrated lipid bilayers.

      PubDate: 2018-02-25T17:58:07Z
      DOI: 10.1016/bs.arnmr.2017.12.003
      Issue No: Vol. 94 (2018)
  • Chapter Four Recent Developments in NMR Studies of Aluminophosphates
    • Authors: Hiroki Nagashima; Charlotte Martineau-Corcos; Grégory Tricot; Julien Trébosc; Frédérique Pourpoint; Jean-Paul Amoureux; Olivier Lafon
      Pages: 113 - 185
      Abstract: Publication date: 2018
      Source:Annual Reports on NMR Spectroscopy, Volume 94
      Author(s): Hiroki Nagashima, Charlotte Martineau-Corcos, Grégory Tricot, Julien Trébosc, Frédérique Pourpoint, Jean-Paul Amoureux, Olivier Lafon
      Aluminophosphate materials include both crystalline and amorphous solids. Microporous crystalline aluminophosphate solids are used for important applications, such as adsorption, gas separation and heterogeneous catalysis. Aluminophosphate glasses are materials employed for technologies, such as high-power laser, sealing glass and radioactive waste storage. Many of their physical and chemical properties (reactivity, adsorption capacity, glass transition, viscosity, …) depend on their atomic-level structure. As a local characterization technique, solid-state NMR provides unique information on the short- and medium-range structures and on motions over timescales spanning many orders of magnitude. In this review, we survey basic and advanced NMR methods, which have been developed and applied for the characterization of aluminophosphate materials. Notably, we discuss NMR techniques to probe connectivities and proximities between identical or distinct nuclei. Finally, we discuss the information on the structure and dynamics provided by solid-state NMR for both crystalline and amorphous aluminophosphate materials.

      PubDate: 2018-02-25T17:58:07Z
      DOI: 10.1016/bs.arnmr.2017.12.004
      Issue No: Vol. 94 (2018)
  • Chapter Five 17O NMR as a Tool in Discrete Metal Oxide Cluster Chemistry
    • Authors: C. André Ohlin; William H. Casey
      Pages: 187 - 248
      Abstract: Publication date: 2018
      Source:Annual Reports on NMR Spectroscopy, Volume 94
      Author(s): C. André Ohlin, William H. Casey
      This chapter covers recent developments in 17O NMR spectroscopy as applied to discrete metal oxide clusters, particularly in the context of their use as models in geochemistry and catalysis. Dynamic 17O NMR methods based on the McConnell–Bloch equations are explored in depth, and recent advances are reviewed. High-pressure NMR methods are also discussed and reviewed, as are recent developments in the use of density functional theory in the computation of 17O NMR shifts in polyoxometalates. The emphasis of the chapter is on the new developments that promise to reinvigorate 17O NMR as a central tool in the study of aqueous chemical kinetics, with the most urgent challenges being understanding the rates of isotopic substitution into bridging oxygens in clusters.

      PubDate: 2018-02-25T17:58:07Z
      DOI: 10.1016/bs.arnmr.2018.01.001
      Issue No: Vol. 94 (2018)
  • Lateral Diffusion and NMR
    • Authors: Peter M. Macdonald; Angel Lai
      Pages: 73 - 111
      Abstract: Publication date: Available online 14 February 2018
      Source:Annual Reports on NMR Spectroscopy
      Author(s): Peter M. Macdonald, Angel Lai
      Lateral diffusion is a fundamental physical property of membrane lipids and proteins. NMR-based lateral diffusion measurements, while avoiding the need for large, rigid fluorophores inherent to fluorescence-based lateral diffusion measurements, must overcome the spectral broadening arising from the slow anisotropic motions in membranes. Two broad categories of techniques have evolved for doing so, one involving pulsed field gradient methods and the second employing exchange spectroscopy methods. How these have been adapted to permit NMR measurements of lateral diffusion in membranes will be described here in the overview, along with the various advantages and limitations of each.

      PubDate: 2018-02-14T17:17:50Z
      DOI: 10.1016/bs.arnmr.2017.12.001
  • NMR Studies of Organic Aerosols
    • Authors: Regina M.B.O. Duarte; João T.V. Matos; Andreia S. Paula; Sónia P. Lopes; Guilherme Pereira; Pérola Vasconcellos; Adriana Gioda; Renato Carreira; Artur M.S. Silva; Armando C. Duarte; Patricia Smichowski; Nestor Rojas; Odon Sanchez-Ccoyllo
      Pages: 513 - 525
      Abstract: Publication date: Available online 26 May 2017
      Source:Annual Reports on NMR Spectroscopy
      Author(s): Regina M.B.O. Duarte, Armando C. Duarte
      Organic aerosols (OAs) composition in the atmosphere is highly complex and strongly influenced by a panoply of sources and different formation processes. Although OAs have been extensively studied in urban, rural, and marine environments, their complexity is still a major obstacle to an improved understanding on how OAs affect the climate and human health. Nuclear magnetic resonance (NMR) spectroscopy has become one of the leading analytical approaches for the characterization of OAs and has gained importance in atmospheric chemistry sciences. This review highlights both solid-state and one- and two-dimensional solution-state NMR spectroscopy as unmatched tools for nontarget structural elucidation of atmospheric OAs. This work aims to demonstrate various applications of NMR in OAs studies, ranging from OAs source apportionment in field studies to investigation of secondary OAs composition in laboratory experiments. The limitations, weaknesses, and major challenges ahead on the application of NMR tools for OAs research are also overviewed.

      PubDate: 2017-05-27T21:55:30Z
      DOI: 10.1016/j.envpol.2017.05.011
      Issue No: Vol. 227 (2017)
  • At Its Extremes: NMR at Giga-Pascal Pressures
    • Authors: Thomas Meier
      Abstract: Publication date: Available online 26 October 2017
      Source:Annual Reports on NMR Spectroscopy
      Author(s): Thomas Meier
      Implementation of nuclear magnetic resonance in high pressure vessels is among the most demanding technological endeavours of the field, owing to inherently low signal amplitudes, low sensitivities of the resonator set-ups, and samples which are both difficult to handle and to access in the finished experimental set-up. The following chapter presents a review of the basic principles of generating pressures in excess of 1GPa (= 10.000atm), followed by a summary of suitable NMR resonators. Additionally, recent high pressure experiments on correlated and uncorrelated electronic system at pressures as high as 30GPa will be covered.

      PubDate: 2017-10-29T00:00:56Z
      DOI: 10.1016/bs.arnmr.2017.08.004
  • Progress in Our Understanding of 19F Chemical Shifts
    • Authors: Jayangika N. Dahanayake; Chandana Kasireddy; Joseph P. Karnes; Rajni Verma; Ryan M. Steinert; Derek Hildebrandt; Olivia A. Hull; Jonathan M. Ellis; Katie R. Mitchell-Koch
      Abstract: Publication date: Available online 16 October 2017
      Source:Annual Reports on NMR Spectroscopy
      Author(s): Jayangika N. Dahanayake, Chandana Kasireddy, Joseph P. Karnes, Rajni Verma, Ryan M. Steinert, Derek Hildebrandt, Olivia A. Hull, Jonathan M. Ellis, Katie R. Mitchell-Koch
      Fluorine NMR spectroscopy has diverse applications, including characterization of chemical reaction mechanisms, protein structure–function studies, and solid-state NMR characterization of crystalline, amorphous, and soft materials. Computational methods have aided in assigning and interpreting chemical shifts, with wide use in solid-state NMR spectroscopy. Work to understand fluorine chemical shifts has been aided by computational methods. So-called “normal” chemical shift behaviour can be understood to arise from ground-state electron density, in which diamagnetic or Lamb shielding dominates. Meanwhile, electronic structure methods indicate that many instances of “reverse” chemical shift behaviour can be understood to be dominated by paramagnetic shielding effects, which arise from the coupling of occupied and unoccupied molecular orbitals in the presence of a magnetic field. Calculations using natural chemical shielding analysis are used to delineate contributions from diamagnetic and paramagnetic shielding of fluorine nuclei in a set of aromatic molecules and aliphatic compounds, some of which exhibit reverse chemical shift behaviour. An overview of recent advances to assign and interpret chemical shifts in complex environments is presented.

      PubDate: 2017-10-21T18:21:42Z
      DOI: 10.1016/bs.arnmr.2017.08.002
  • Perspective on the Hyperpolarisation Technique Signal Amplification by
           Reversible Exchange (SABRE) in NMR Spectroscopy and MR Imaging
    • Authors: Thomas B.R. Robertson; Ryan E. Mewis
      Abstract: Publication date: Available online 16 October 2017
      Source:Annual Reports on NMR Spectroscopy
      Author(s): Thomas B.R. Robertson, Ryan E. Mewis
      Signal amplification by reversible exchange (SABRE) is a para-hydrogen-based technique that utilises a metal complex, normally centred on iridium, to propagate polarisation from para-hydrogen-derived hydride ligands to spin-½ nuclei located in a bound substrate. To date, substrates possessing 1H, 13C, 15N, 19F, 31P, 29Si, and 119Sn nuclei have been polarised by this technique. The exact positioning of these nuclei has a direct bearing on the enhancement observed and so substrates must be chosen or synthesised with care in order to maximise polarisation transfer, and hence the resulting enhancement. The chemical composition of the metal complex must be similarly appraised, as the exchange rate of substrates and para-hydrogen is implicated heavily in efficient polarisation transfer. The nature of the polarisation transfer, whether homogenous or heterogeneous, is another important facet to consider here, as is conducting SABRE in water-based systems. This review discusses the physical and theoretical aspects of the SABRE experiment, as well as the applications of the SABRE technique, namely, the detection of analytes at concentrations far below what would be possible with conventional NMR techniques and the collection of hyperpolarised magnetic resonance images. Advances relating to utilising singlet states for SABRE, pulse sequence design and the nature of the polarisation transfer mechanism are also discussed, and the implications for future SABRE-based discoveries highlighted.

      PubDate: 2017-10-21T18:21:42Z
      DOI: 10.1016/bs.arnmr.2017.08.001
  • Ultrafast 2D NMR: Methods and Applications
    • Authors: Boris Gouilleux; Laetitia Rouger; Patrick Giraudeau
      Abstract: Publication date: Available online 16 October 2017
      Source:Annual Reports on NMR Spectroscopy
      Author(s): Boris Gouilleux, Laetitia Rouger, Patrick Giraudeau
      Multidimensional NMR (nD NMR) has become one of the most powerful spectroscopic tools to deliver diverse structural and functional insights into organic and biomolecules as well as on raw materials. A long-standing concern of nD NMR is related to its long experiment duration, arising from the need to sample the indirect dimension(s) in a multistep fashion. For decades, the NMR community has been developing numerous strategies to speed up nD NMR experiments and therefore extend their scope of applications. Among them is the ultrafast (UF) NMR methodology, capable of delivering arbitrary homo- or heteronuclear multidimensional spectra in a single scan. Since the initial concept was published in 2002, the performance of this subsecond 2D NMR approach has been greatly improved so that UF NMR is nowadays a relevant analytical tool used in broad variety of situations whereby the experiment duration is crucial. Following a description of the principles of UF NMR, the present review aims at emphasizing the numerous methodological developments that this approach has undergone so far in 2017. Thereafter, the high versatility of UF NMR is highlighted through the review of the applications that have been reported in a variety of settings and disciplines, in isotropic as well as anisotropic media.

      PubDate: 2017-10-21T18:21:42Z
      DOI: 10.1016/bs.arnmr.2017.08.003
  • Recent Advances in 11B Solid-State Nuclear Magnetic Resonance Spectroscopy
           of Crystalline Solids
    • Authors: Ying-Tung Angel Wong; David L. Bryce
      Abstract: Publication date: Available online 16 October 2017
      Source:Annual Reports on NMR Spectroscopy
      Author(s): Ying-Tung Angel Wong, David L. Bryce
      We review the progress made in 11B solid-state nuclear magnetic resonance (SSNMR) spectroscopy of crystalline materials over the past 20 years, with a focus on the applications of 11B NMR observables in providing electronic and structural information. A brief description of some of the common SSNMR methods for measuring 11B chemical shift (CS) tensor parameters, electric field gradient (EFG) tensor parameters, and indirect spin–spin (J) coupling constants is first provided. Recent 11B SSNMR studies on crystalline boron systems, such as diboron compounds, boronic esters and acids, borates, and boron-containing Lewis acid/base adducts, are then summarized, and the corresponding experimentally obtained 11B NMR parameters are presented. In general, data from studies that only report isotropic CSs are not tabulated. Our survey highlights the ability of 11B SSNMR spectroscopy to provide an abundance of diverse chemical information, ranging from the coordination environment of the boron, to ligand identity, bond strengths, bond orders and bond angles, and the potential of this technique to characterize inorganic and organic crystalline solids. Owing to the sensitivity of 11B SSNMR spectroscopy to chemical structures and the suitability of the 11B nuclide for high-resolution techniques such as MQMAS and DOR, we anticipate that 11B SSNMR spectroscopy will continue to evolve as an indispensable tool for solid-state characterization of boron-containing systems and for the advancement of various fields, such as NMR crystallography, the synthesis of novel boron reagents, and the development of boron-based hydrogen storage materials.

      PubDate: 2017-10-21T18:21:42Z
      DOI: 10.1016/bs.arnmr.2017.08.005
  • Recent NMR Studies of Thermoelectric Materials
    • Authors: Ali A. Sirusi; Joseph H. Ross
      Abstract: Publication date: Available online 16 June 2017
      Source:Annual Reports on NMR Spectroscopy
      Author(s): Ali A. Sirusi, Joseph H. Ross
      Thermoelectric materials can directly convert heat to electricity and are expected to lead to new devices to harvest waste heat for energy efficiency as well as new cooling technologies. Optimization of these properties requires tailoring vibrational properties as well as the entropy carried by electrical charges and spins. NMR measurements have been important for understanding these processes, providing a measure of anharmonic “rattling” phonon behavior, local fluctuations in charge carrier and magnetic properties, and atomic-scale symmetries and distortions within these materials. Here we report recent NMR results focusing on inorganic clathrates, skutterudites, oxides, noble metal chalcogenides, complex tellurides, and half-Heusler compounds in which high thermoelectric efficiencies have been reported.

      PubDate: 2017-08-04T10:41:15Z
      DOI: 10.1016/bs.arnmr.2017.04.002
  • Applications of Solid-State 43Ca Nuclear Magnetic Resonance:
           Superconductors, Glasses, Biomaterials, and NMR Crystallography
    • Authors: Cory M. Widdifield
      Abstract: Publication date: Available online 10 July 2017
      Source:Annual Reports on NMR Spectroscopy
      Author(s): Cory M. Widdifield
      The application of 43Ca solid-state nuclear magnetic resonance (SSNMR) experiments to probe various materials is reviewed. Methods used to obtain high-quality 43Ca SSNMR spectra, and the types of information which can be gained by recording 43Ca NMR spectra, are outlined. Substantial discussion is provided in relation to the classes of materials which have already been studied, at least in part, by 43Ca SSNMR. This includes, but is not limited to, superconductors, binary and ternary calcium-containing inorganics (and hydrates thereof), silicates, glasses, cements, concretes, clays, phosphates, bones, teeth, calcium-containing organics, and biomaterials. Studies that include the computation of calcium NMR parameters using quantum chemistry methods are discussed in detail, which leads naturally to accounts pertaining to NMR crystallography. This review concludes with brief speculations on the future of 43Ca SSNMR.

      PubDate: 2017-07-19T08:27:27Z
      DOI: 10.1016/bs.arnmr.2017.04.006
  • Nonlinear Effects in NMR
    • Authors: Matthias Bechmann; Norbert Müller
      Abstract: Publication date: Available online 23 June 2017
      Source:Annual Reports on NMR Spectroscopy
      Author(s): Matthias Bechmann, Norbert Müller
      Analytical applications of NMR exploit the widely assumed linearity of the NMR response with respect to the spin concentration. Deviations of this linearity are undesired and in this review some current approaches to tackle this problem are given. However, from a physics point of view, the nonlinearity is a more complex affair. Indeed, NMR as a primary representative of coherent spectroscopy can be viewed as an inherently nonlinear method, in particular with respect to the excitation amplitude. Even excluding this intrinsic property, amplitude response is not always found to be linear and several distinct fundamental nonlinearity or nonadditivity effects can be caused by spin interactions, which can either be internal to the specimen, or owed to feedback from the observation electronics as summarized here with references to the latest literature. Ways to avoid nonlinear response for quantitative NMR applications are summarized briefly.

      PubDate: 2017-06-29T10:47:28Z
      DOI: 10.1016/bs.arnmr.2017.04.005
  • Solid-State NMR Spectroscopy: The Magic Wand to View Bone at Nanoscopic
    • Authors: Kamal H. Mroue; Akhila Viswan; Neeraj Sinha; Ayyalusamy Ramamoorthy
      Abstract: Publication date: Available online 7 June 2017
      Source:Annual Reports on NMR Spectroscopy
      Author(s): Kamal H. Mroue, Akhila Viswan, Neeraj Sinha, Ayyalusamy Ramamoorthy
      The unique potential of solid-state NMR (SSNMR) spectroscopy to provide atomistic-scale piercing insights into the structure and dynamics of complex biomaterials, such as the extracellular matrix of bone and related connective tissues, has been well demonstrated over the past several years. With its highly complex hierarchical architecture, bone indeed represents a significant challenge to structural studies using many conventional analytical and biophysical techniques. Recent instrumental and technological advances have considerably improved the sensitivity and resolution in multidimensional magic-angle spinning SSNMR experiments and have made it possible to obtain key high-resolution information, that are otherwise unobtainable by conventional microscopic and diffraction studies, from insoluble and amorphous heterogeneous materials of biological importance such as bone. In this review, we briefly present recent and continuing advances in the area of SSNMR of bone and related connective tissues like cartilage, by summarizing a selected ensemble of key SSNMR applications that highlight the potential with which this technique has contributed to our growing understanding of the complex structures and dynamics of these materials.

      PubDate: 2017-06-12T09:46:20Z
      DOI: 10.1016/bs.arnmr.2017.04.004
  • The DEPT Experiment and Some of Its Useful Variants
    • Authors: Hedvika Primasova; Peter Bigler; Julien Furrer
      Abstract: Publication date: Available online 1 June 2017
      Source:Annual Reports on NMR Spectroscopy
      Author(s): Hedvika Primasova, Peter Bigler, Julien Furrer
      The DEPT (distortionless enhancement by polarization transfer) experiment, proposed in 1982, has revolutionized NMR spectroscopy for signal assignment, particularly for obtaining information with respect to, e.g., the type (multiplicity) and the number of Cq, CH, CH2, and CH3 in the investigated molecule and for calculating corresponding carbon type-specific subspectra (spectral editing). In this chapter, we have explored various DEPT pulse sequences and have discussed how the pulse sequence elements cooperate and contribute to the final shape and appearance of the observed signals. In addition, we have compared the results with other experiments designed for the determination of multiplicities like the spin echo (SE)-based experiments SEFT, APT, and SEMUT, and the experiments where the signal intensity is enhanced by heteronuclear polarization transfer such as the INEPT-based experiments INEPT and PENDANT, and the DEPT-based experiments DEPT, POMMIE, and DEPTQ. After a short introduction, this chapter, with the aid of product operator formalism, provides a comprehensive description of these experiments. Building from basic principles, the DEPTQ variant, for including the signals of quaternary carbons, the ACCORDEPT, for equalizing intensities in case of a wide range of heteronuclear coupling constants, and the QDEPT and QDEPT+ sequences, for obtaining quantitative DEPT data are explained in detail.

      PubDate: 2017-06-07T09:29:22Z
      DOI: 10.1016/bs.arnmr.2017.04.001
  • MRI Studies of Plastic Crystals
    • Authors: K. Romanenko
      Abstract: Publication date: Available online 9 February 2017
      Source:Annual Reports on NMR Spectroscopy
      Author(s): K. Romanenko
      Over three decades ago, plastic crystals were proposed as a solid-state alternative to conventional liquid electrolytes. Particular attention has been later drawn to organic ionic plastic crystals (OIPCs) and OIPC-based electrolytes. These ionic solids exhibit crucial characteristics of a safe electrolyte material such as nonflammability, nonvolatility, electrochemical stability, and plasticity. Versatility of ionic pairs available to date and ongoing research on molecular design will provide OIPCs for specific operating conditions within a broad range of electrochemical applications. Single-point ramped imaging with T 1 enhancement (SPRITE), an MRI method known for its capability to visualize solids, has played a key role in the discovery of several novel phenomena inherent in OIPCs. This chapter is an overview of these solid-state MRI studies. SPRITE imaging of polycrystalline morphology revealed a striking T 2 * contrast anisotropy and shed light on molecular dynamics in solid phases of plastic crystals. These observations suggest the possibility of macroscopically anisotropic ion conduction supported by impedance spectroscopy and in situ MRI experiments. MRI studies of operating electrochemical cells have led to a breakthrough in understanding the function of doped plastic crystals. The discovered hybrid solid–liquid property of OIPC electrolytes is the key for their successful commercialization.

      PubDate: 2017-02-10T08:20:40Z
      DOI: 10.1016/bs.arnmr.2016.12.002
  • Magnetic Resonance Imaging Studies of the Spatial Distribution of Charge
    • Authors: K. Borzutzki; G. Brunklaus
      Abstract: Publication date: Available online 6 February 2017
      Source:Annual Reports on NMR Spectroscopy
      Author(s): K. Borzutzki, G. Brunklaus
      Charge carriers are an essential component of electrochemical devices or participants in redox processes and govern the achievable properties or performance of the considered materials. Since well-defined structural features of active components including the explicit coordination sphere of charge carriers typically exists at rather locale scale, the application of methods that require long-range order reflecting crystalline lattices such as X-ray diffraction is limited. In this context, magnetic resonance imaging (MRI) constitutes a highly viable option as MRI (or more general NMR) is element selective, hence, charge carrier specific and able to tolerate ill-defined structural arrangements. A skillful combination of available MRI methods allows for monitoring of electrochemical processes with sufficient spatial and temporal resolution, and their recent applications in the field of batteries and other redox chemistry are concisely summarized and discussed in this review.

      PubDate: 2017-02-10T08:20:40Z
      DOI: 10.1016/bs.arnmr.2016.12.003
  • Novel Synthetic As Well As Natural Auxiliaries With a Blend of NMR
           Methodological Developments for Chiral Analysis in Isotropic Media
    • Authors: Sandeep K. Mishra; Sachin R. Chaudhari; A. Lakshmipriya; Indrani Pal; N. Lokesh; N. Suryaprakash
      Abstract: Publication date: Available online 24 January 2017
      Source:Annual Reports on NMR Spectroscopy
      Author(s): Sandeep K. Mishra, Sachin R. Chaudhari, A. Lakshmipriya, Indrani Pal, N. Lokesh, N. Suryaprakash
      Chiral auxiliaries are routinely employed in the NMR spectroscopic discrimination of enantiomers in isotropic solutions. Most of the times the presence of impurities, superposition of peaks, enormous line broadening, and complex multiplicity pattern limit the NMR spectroscopic discrimination of enantiomers and determination of their composition. There are a few approaches to unravel the overlap of peaks. A simple approach is to utilize appropriate chiral auxiliary, which induces a large chemical shift difference between the discriminated peaks (Δδ) R/S , and minimize or unravel the overlap of peaks. In this direction, several new chiral auxiliaries and new chiral differentiation protocols have been introduced, which are both synthetic and naturally occurring molecules. An alternate spectroscopic approach is to design NMR experiments to circumvent inherent problems, viz., enhancing the spectral resolution, separation of the superimposed spectra of enantiomers, and reduction of the spectral complexity. A large number of NMR experiments, such as two-dimensional selective F 1 decoupling, RES-TOCSY, multiple quantum detection, frequency-selective homodecoupling, band-selective homodecoupling, and broadband homodecoupling called as pure shift NMR, to cite a few, are available for such a purpose. Many of these techniques have simplified the chiral analysis for molecules containing diverse functional groups in the presence of suitable chiral auxiliaries. The present chapter summarizes the work carried out in the authors’ laboratory on chiral analysis. This includes the recently introduced new chiral auxiliaries, which are either synthesizable or natural products. They could be either derivatizing agents or solvating agents or the developed three-component protocols, in addition to new NMR experimental methodologies.

      PubDate: 2017-01-29T08:11:07Z
      DOI: 10.1016/bs.arnmr.2016.12.001
  • NMR Relaxation in Dendrimers
    • Authors: D.A. Markelov; M. Dolgushev; E. Lähderanta
      Abstract: Publication date: Available online 9 January 2017
      Source:Annual Reports on NMR Spectroscopy
      Author(s): D.A. Markelov, M. Dolgushev, E. Lähderanta
      This review focuses on recent advances in the theory of local orientational mobility in dendrimers that reveals in the NMR relaxation. In particular, we summarize recent results of analytic theory, computer simulations, and NMR relaxation experiments. The analytic theory provides basic means for the analysis of the simulations and experiments by predicting the existence of two dominating processes: overall branch relaxation and local vibrations. On the other hand, the results of simulations and experiments complete the picture by a third process of rotation of the dendrimer as a whole. The NMR relaxation reveals a fundamental importance of the local constraints on segments’ orientations. Remarkably, the model, in which such constraints are absent, overestimates local vibrations making the NMR relaxation rate functions for segments that have different topological location in the dendrimer to be practically indistinguishable. Inclusion of the bending rigidity fixes this flaw by endorsing the process of overall branch relaxation. This leads to a correct recognition of the slower mobility of the segments that are located closer to the dendrimer's core. The crucial role of the local constraints for the NMR relaxation functions is supported by a series of experiments and simulations.

      PubDate: 2017-01-15T07:52:15Z
      DOI: 10.1016/bs.arnmr.2016.11.001
  • Recent MRI and Diffusion Studies of Food Structures
    • Authors: D. Groß; K. Zick; G. Guthausen
      Abstract: Publication date: Available online 31 October 2016
      Source:Annual Reports on NMR Spectroscopy
      Author(s): D. Groß, K. Zick, G. Guthausen
      Food is an essential class of materials for animal and human beings and deserves closer scientific attention. In the context of magnetic resonance imaging (MRI) and diffusion measured by nuclear magnetic resonance (NMR), mainly structural and compositional aspects can be addressed to study natural food systems with the aim of a deeper and comprehensive description but also to study processes applied to foods and the final products. In this review the currently available and in the context of foods applied MRI and diffusion NMR methods are summarized together with examples of their applications.

      PubDate: 2016-11-03T02:11:49Z
      DOI: 10.1016/bs.arnmr.2016.09.001
  • NMR Studies of Fossilized Wood
    • Authors: M. Bardet; A. Pournou
      Abstract: Publication date: Available online 15 September 2016
      Source:Annual Reports on NMR Spectroscopy
      Author(s): M. Bardet, A. Pournou
      Fossil wood represents an exceptional and challenging material for nuclear magnetic resonance (NMR) investigation, as it embodies an intriguing multicompound chemistry and a complex and multifarious morphology. This rare plant remain, which managed to escape recycling, can offer through the various NMR applications a valuable contribution to the understanding of the biogeochemistry of wood fossilization. Furthermore, via NMR analysis, key issues of taphonomy, paleoecology, and plants’ evolutionary history can be investigated, providing significant inputs to the science of paleontology. This review commences with the three main forms of fossilized wood, coalified, petrified, and mummified and the respective fossilization mechanisms. Then, it presents various NMR applications and provides some fundamental features of NMR itself such as (a) the appropriate nuclei that can be employed, (b) important aspects of solid-state 13C NMR, (c) differences of 1D and 2D experiments and sequences, (d) the potential of quantitative analysis, (e) advantages of combining NMR with microscopy, and (f) some emerging NMR techniques such as the dynamic nuclear polarization solid-state NMR and the microimaging NMR. The main purpose of this work is to introduce the general principles required for a reliable and reproducible analysis of fossil wood with NMR. Additionally, it aims to present the range of research possibilities arising from NMR investigation and their expected outcomes. Finally, it anticipates that it can be a starting point for further research on fossilized wood and a motivation for developing innovative NMR applications.

      PubDate: 2016-09-21T15:38:06Z
      DOI: 10.1016/bs.arnmr.2016.07.002
  • Quantitative NMR Studies of Multiple Compound Mixtures
    • Abstract: Publication date: Available online 12 September 2016
      Source:Annual Reports on NMR Spectroscopy
      Author(s): X. Li, K. Hu
      The unique analytical capabilities of both identification and quantification of compounds in complex mixture by NMR technique have been demonstrated. qNMR is widely applied as routine analytical tool for the mixtures because of the universal existence of NMR-active nuclei. qNMR is one of the few standard-free quantification methods. It can quantitatively analyze multiple compound mixtures without requirement of chemical identical standards. In this review, theoretic background and technical keynotes on qNMR data acquisition, spectral processing, and signal deconvolution/integration will be discussed for quantitative analysis of multiple compound mixtures. Sample preparation and the effect of different sample conditions on the assessment of the concentration will also be discussed. 1H 1D qNMR is the most often used method for quantitative analysis of multiple compound mixtures, yet heteronuclear 1D and 2D qNMR approaches have been increasingly recognized and exploited for quantitative assessment or concentration measurement. Some often used quantitative NMR methods are then summarized. Afterwards, applications of qNMR in the areas of metabolomics, natural products, traditional Chinese herbal medicine (TCM), pharmaceutical research and food analysis are exemplified. Finally, we prospect the future developments and applications of qNMR.

      PubDate: 2016-09-21T15:38:06Z
  • The Chemical Bond: The Perspective of NMR Spectroscopy
    • Abstract: Publication date: Available online 1 September 2016
      Source:Annual Reports on NMR Spectroscopy
      Author(s): M. Dračínský
      This review article deals with chemical bonding from the perspective of nuclear magnetic resonance (NMR) spectroscopy. Different types of chemical bonds are briefly discussed and the relation between chemical bonding and NMR observables is overviewed. The various NMR interactions are classified in terms of through-bond and through-space effects on their observable values. The effects of vibrational motion and nuclear delocalization on NMR parameters and the consequences for the experimental determination of bond distances are also discussed. Finally, NMR experiments in studies of hydrogen bonding are summarized in Section 5.

      PubDate: 2016-09-21T15:38:06Z
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