Sensitivity and Resolution Enhancement of Half-integer Quadrupolar Nuclei in Solid-state NMR

Nakashima, Thomas T.; Wasylishen, Roderick E.

doi:10.1002/9780470034590.emrstm1200

Cited by 5 publications

(5 citation statements)

References 43 publications

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“…However, MQMAS suffers from poor sensitivity, owing to the use of a formally "forbidden" multiple-quantum transition. While much effort has been devoted to developing pulse schemes [35][36][37] to improve the sensitivity of the experiment, the related satellite transition (ST) MAS experiment [6,38,39] offers much higher inherent sensitivity (owing to the use of only allowed single-quantum transitions throughout the experiment), albeit at the cost of a more exacting experimental setup in terms of MAS stability and the precision of the magic angle setting. Both experiments are, however, typically preferred to the one-dimensional DOR technique discussed above, as there is no need for specialist hardware.…”

Section: Experimental Methodologymentioning

confidence: 99%

Exploiting NMR spectroscopy for the study of disorder in solids

Moran

Dawson

Ashbrook

2017

International Reviews in Physical Chemistry

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Although the solid state is typically characterised by inherent periodicity, many interesting physical and chemical properties of solids arise from a variation in this, i.e., changes in the nature of the atom occupying a particular site in a crystal structure or variation in the position of an atom (or group of atoms) in different parts of a structure, or variation as a function of time. This lack of long-range order poses significant challenges, not just for the characterisation of the structure of disordered materials, but also simply for its description. The sensitivity of nuclear magnetic resonance (NMR) spectroscopy to the local, atomic-scale environment, without the requirement for long-range order, makes it a powerful tool for the study of disorder in the solid state. Information on the number and type(s) of coordinating atoms or through-space and through-bond connectivity between atomic species enables the construction of a detailed picture of the structure. After a brief description of the background theory of NMR spectroscopy, and the experimental methods employed, we will describe the effects of disorder on NMR spectra and the use of calculations to help interpret experimental measurements. We will then review a range of applications to different types of disordered materials, including oxides and ceramics, minerals, porous materials, biomaterials, energy materials, pharmaceuticals, polymers and glasses. We will discuss the most successful approaches for studying different materials, and illustrate the type of information available and the structural insight gained.

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Section: Experimental Methodologymentioning

confidence: 99%

Exploiting NMR spectroscopy for the study of disorder in solids

Moran

Dawson

Ashbrook

2017

International Reviews in Physical Chemistry

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“…For wideline experiments, sensitivity is a particular challenge, and many approaches have been used to overcome this, including Carr–Purcell–Meiboom–Gill (CPMG) echo trains and manipulation of the population of the nuclear energy levels using FAM-type pulses, double frequency sweep (DFS) pulses, or shaped hyperbolic secant (HS) pulses. , Most of the approaches used are equally applicable to rotating samples and can be employed in conventional MAS experiments. References and provide more detail in this area.…”

Section: Background and Basic Experimentsmentioning

confidence: 99%

“…In addition to the challenges faced for inorganic solids, there are often relatively few metal sites in biological systems, and many of the relevant species have low receptivities and/or significant quadrupolar broadening. This emerging area, therefore, had been facilitated more than most by the use of higher magnetic fields, advances in hardware, and the introduction of sensitivity enhancement schemes. , …”

Section: Recent Applications Of Solid-state Nmr Spectroscopy Of Quadr...mentioning

confidence: 99%

“…This emerging area, therefore, had been facilitated more than most by the use of higher magnetic fields, advances in hardware, and the introduction of sensitivity enhancement schemes. 14,33 It has been estimated that at least one-third of all proteins and enzymes that have been purified require metals for their biological function. 14 One such example is zinc-containing proteins, where the metal center plays an important role in structure and catalysis.…”

Section: Recent Applications Of Solid-state Nmrmentioning

confidence: 99%

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New Methods and Applications in Solid-State NMR Spectroscopy of Quadrupolar Nuclei

2014

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Solid-state nuclear magnetic resonance (NMR) spectroscopy has long been established as offering unique atomic-scale and element-specific insight into the structure, disorder, and dynamics of materials. NMR spectra of quadrupolar nuclei (I > (1)/2) are often perceived as being challenging to acquire and to interpret because of the presence of anisotropic broadening arising from the interaction of the electric field gradient and the nuclear electric quadrupole moment, which broadens the spectral lines, often over several megahertz. Despite the vast amount of information contained in the spectral line shapes, the problems with sensitivity and resolution have, until very recently, limited the application of NMR spectroscopy of quadrupolar nuclei in the solid state. In this Perspective, we provide a brief overview of the quadrupolar interaction, describe some of the basic experimental approaches used for acquiring high-resolution NMR spectra, and discuss the information that these spectra can provide. We then describe some interesting recent examples to showcase some of the more exciting and challenging new applications of NMR spectra of quadrupolar nuclei in the fields of energy materials, microporous materials, Earth sciences, and biomaterials. Finally, we consider the possible directions that this highly informative technique may take in the future.

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“…Further improvements in sensitivity are typically required for the acquisition of wideline spectra, and techniques such as CPMG (Carr Purcell Meiboom Gill) echo trains in acquisition (as used in Figure 2c), or the prior manipulation the population of the nuclear spin energy levels, are routinely employed. (36) Sensitivity enhancement techniques are discussed in Section 3 below.…”

Section: Advanced Methodology and Challenging Systemsmentioning

confidence: 99%

Recent Advances in Solid-State Nuclear Magnetic Resonance Spectroscopy

Ashbrook

Griffin

Johnston

2018

Annual Rev. Anal. Chem.

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The sensitivity of nuclear magnetic resonance (NMR) spectroscopy to the local atomic-scale environment offers great potential for the characterization of a diverse range of solid materials. Despite offering more information than its solution-state counterpart, solid-state NMR has not yet achieved a similar level of recognition, owing to the anisotropic interactions that broaden the spectral lines and hinder the extraction of structural information. Here, we describe the methods available to improve the resolution of solid-state NMR spectra and the continuing research in this area. We also highlight areas of exciting new and future development, including recent interest in combining experiment with theoretical calculations, the rise of a range of polarization transfer techniques that provide significant sensitivity enhancements, and the progress of in situ measurements. We demonstrate the detailed information available when studying dynamic and disordered solids and discuss the future applications of solid-state NMR spectroscopy across the chemical sciences.

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Sensitivity and Resolution Enhancement of Half-integer Quadrupolar Nuclei in Solid-state NMR

Cited by 5 publications

References 43 publications

Exploiting NMR spectroscopy for the study of disorder in solids

Exploiting NMR spectroscopy for the study of disorder in solids

New Methods and Applications in Solid-State NMR Spectroscopy of Quadrupolar Nuclei

Recent Advances in Solid-State Nuclear Magnetic Resonance Spectroscopy

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