Solid-State NMR at 850 MHz: A World-leading UK Facility to deliver Advances in Materials Science, Chemistry, Biology, Earth Science and Physics
Lead Research Organisation:
University of Warwick
Department Name: Physics
Abstract
It is the structural arrangement and motion of molecules and ions that determine, e.g., the bulk properties of a material or the function of biomolecules. Therefore, the availability of state-of-the-art analytical infrastructure for probing atomic-level structure and dynamics is essential to enable advances across science. The power of solid-state Nuclear Magnetic Resonance (NMR) as such a probe is being increasingly demonstrated by applications to, e.g., materials for hydrogen storage and radioactive waste encapsulation, pharmaceutical formulations, and the amyloid plaques associated with diseases such as Alzheimer's. Solid-state NMR is most sensitive to the local chemical structure (usually up to a few bond lengths) around a particular nucleus and is thus well suited to characterising the many important systems that lack periodic order, making it complementary to well-established diffraction techniques.To extend the applicability of NMR, two key limiting factors must be addressed: sensitivity, i.e., the relative intensity of spectral peaks as compared to the noise level, and resolution, i.e., the linewidths of individual peaks that determine whether two close-together signals can be separately observed. Both sensitivity and resolution are much improved by performing NMR experiments at higher magnetic field, thus making possible applications that are not feasible at lower field. Hence, this proposal is to establish a UK facility for solid-state NMR at a world-leading magnetic field strength of 20 Tesla, corresponding to a frequency for the 1H hydrogen nucleus of 850 MHz. The resonant frequency of different nuclear isotopes are well separated such that an NMR spectrum is specific to a particular chosen isotope. NMR experiments at 20 Tesla will make use of as much of the Periodic Table as possible. A particular focus will be on nuclei which are difficult due to their low natural abundance or low resonance frequency - there are many important so-called low-gamma nuclei, e.g., 25Mg, 33S, 39K, 43Ca, 47/49Ti, with resonance frequencies < 10% of 1H. High magnetic field is especially important for the study of the over two thirds of NMR-active isotopes (i.e., with non-zero spin) that possess a quadrupolar electric moment, i.e., a non-spherical distribution of electric charge. For nuclei with spin 1/2, e.g., 13C, the routinely applied technique of physically rotating the sample around an axis inclined at the so-called magic angle of 54.7 degrees to the magnetic field direction yields narrow resonance peaks. However, for the many quadrupolar nuclei with half-integer spin, a residual broadening remains in the magic-angle spinning experiment. This residual quadrupolar broadening (in the usual NMR scale of ppm) is inversely proportional to the magnetic field squared; as well as improving resolution, the concentration of the signal intensity into a narrower lineshape hence means a still greater sensitivity dependence on the magnetic field strength. Oxygen is a key constituent of most organic and inorganic compounds; however, it is difficult to study by NMR since the only NMR-active isotope is the quadrupolar nucleus 17O, whose natural abundance is only 0.037 %. Nearly all NMR studies to date have required the preparation of 17O-labelled samples (starting with 17O-enriched water); very excitingly, working at 20 Tesla offers the possibility of recording high-resolution 17O spectra at natural abundance.A test of a powerful technique is its applicability to a wide range of problems. The high-field solid-state NMR facility will make possible experiments that provide unique information for applications across science, ranging from materials for catalysis, radioactive waste encapsulation, dental implants, batteries, drug delivery, through gaining new understanding of geological processes, to the life sciences, e.g., amyloid plaques, metal-binding proteins, bone structure, membrane proteins, enzymes.
Publications
Johnston KE
(2011)
93Nb NMR and DFT investigation of the polymorphs of NaNbO3.
in Physical chemistry chemical physics : PCCP
Iwama S
(2014)
Highly efficient chiral resolution of DL-arginine by cocrystal formation followed by recrystallization under preferential-enrichment conditions.
in Chemistry (Weinheim an der Bergstrasse, Germany)
Iuga D
(2014)
A 3D experiment that provides isotropic homonuclear correlations of half-integer quadrupolar nuclei.
in Journal of magnetic resonance (San Diego, Calif. : 1997)
Iuga D
(2011)
Double-quantum homonuclear correlations of spin I=5/2 nuclei.
in Journal of magnetic resonance (San Diego, Calif. : 1997)
Inglis K
(2016)
Structure and Sodium Ion Dynamics in Sodium Strontium Silicate Investigated by Multinuclear Solid-State NMR
in Chemistry of Materials
Hughes CE
(2014)
"CLASSIC NMR": an in-situ NMR strategy for mapping the time-evolution of crystallization processes by combined liquid-state and solid-state measurements.
in Angewandte Chemie (International ed. in English)
Hughes CE
(2015)
New in situ solid-state NMR techniques for probing the evolution of crystallization processes: pre-nucleation, nucleation and growth.
in Faraday discussions
Hughes CE
(2012)
Exploiting In Situ Solid-State NMR for the Discovery of New Polymorphs during Crystallization Processes.
in The journal of physical chemistry letters
Howes AP
(2011)
Boron environments in Pyrex® glass--a high resolution, Double-Rotation NMR and thermodynamic modelling study.
in Physical chemistry chemical physics : PCCP
Harris KD
(2015)
Monitoring the evolution of crystallization processes by in-situ solid-state NMR spectroscopy.
in Solid state nuclear magnetic resonance
Harris K
(2016)
New in situ solid-state NMR strategies for exploring materials formation and adsorption processes: prospects in heterogenous catalysis
in Applied Petrochemical Research
Haies IM
(2015)
(14)N overtone NMR under MAS: signal enhancement using symmetry-based sequences and novel simulation strategies.
in Physical chemistry chemical physics : PCCP
Grigg A
(2015)
Vitrification of ß-tricalcium phosphate in sodium aluminoborophosphate glass and the effect of Ga3+ substitution
in Journal of Solid State Chemistry
Grigg A
(2014)
Cation substitution in ß-tricalcium phosphate investigated using multi-nuclear, solid-state NMR
in Journal of Solid State Chemistry
Griffin JM
(2011)
Observation of "hidden" magnesium: first-principles calculations and 25Mg solid-state NMR of enstatite.
in Solid state nuclear magnetic resonance
Griffin J
(2012)
Ionothermal 17O enrichment of oxides using microlitre quantities of labelled water
in Chemical Science
Griffin J
(2013)
Water in the Earth's mantle: a solid-state NMR study of hydrous wadsleyite
in Chemical Science
Gras P
(2016)
From crystalline to amorphous calcium pyrophosphates: A solid state Nuclear Magnetic Resonance perspective.
in Acta biomaterialia
Gardner L
(2015)
Characterisation of magnesium potassium phosphate cements blended with fly ash and ground granulated blast furnace slag
in Cement and Concrete Research
Frantsuzov I
(2017)
Rationalising Heteronuclear Decoupling in Refocussing Applications of Solid-State NMR Spectroscopy.
in Chemphyschem : a European journal of chemical physics and physical chemistry
Fauré N
(2013)
A Solid-State NMR Study of the Immobilization of a-Chymotrypsin on Mesoporous Silica
in The Journal of Physical Chemistry C
Enciso-Maldonado L
(2015)
Computational Identification and Experimental Realization of Lithium Vacancy Introduction into the Olivine LiMgPO 4
in Chemistry of Materials
Eills J
(2018)
Preservation of Nuclear Spin Order by Precipitation.
in Chemphyschem : a European journal of chemical physics and physical chemistry
Duer MJ
(2015)
The contribution of solid-state NMR spectroscopy to understanding biomineralization: atomic and molecular structure of bone.
in Journal of magnetic resonance (San Diego, Calif. : 1997)
Description | The grant established the UK 850 MHz Solid-State NMR Facility (now an EPSRC National Research Facility): operational since 2010, this is based around a wide-bore 20 T (or 850 MHz) NMR spectrometer, together with a range of specialised probes, supported by a dedicated Facility Manager and overseen by a Facility Executive and Oversight Committee. Up to the end of this initial grant in 2015, the Facility had been used by 47 distinct PIs from 22 different UK institutions. Access by the UK scientific community to the 850 MHz Solid-State NMR Facility has provided new insight for a wide range of application areas of economic and social importance: (i) chemistry, e.g., pharmaceuticals, self-assembled nanostructures, crystallisation phenomena (ii) materials science, e.g., batteries, catalysts, hydrogen storage and motion, metal-organic frameworks, carbon capture, cement, tissue scaffolds, storage of nuclear waste (iii) biology, e.g., plant cell walls, protein complexes, membrane proteins, bone and biomineral structure Industry has accessed the state-of-the-art solid-state NMR instrumentation either via either via paid-for industrial contract research or through industry support of PhD student users of the Facility, for example, the pharmaceutical (e.g., AstraZeneca and GlaxoSmithKline), oil/ fuel (e.g., Infineum and Sasol) and catalysis/ materials (e.g., BP, Johnson Matthey) industry. The Facility also provides the opportunity for users to share implemented NMR pulse sequences for the benefit of the wider community. |
Exploitation Route | As examples, specific case studies have been prepared for: 1. NMR Crystallography in Pharmaceutical Development 2. Molecular architecture of plant cell walls 3. NMR spectroscopy of microporous materials 4. Large protein complexes by fast MAS NMR https://warwick.ac.uk/fac/sci/physics/research/condensedmatt/nmr/850/case_studies/ |
Sectors | Agriculture, Food and Drink,Chemicals,Energy,Healthcare,Manufacturing, including Industrial Biotechology,Pharmaceuticals and Medical Biotechnology |
URL | https://warwick.ac.uk/fac/sci/physics/research/condensedmatt/nmr/850/annual_reports/ |
Description | Access by the UK scientific community to the 850 MHz Solid-State NMR Facility has provided new insight for a wide range of application areas of economic and social importance: (i) chemistry, e.g., pharmaceuticals, self-assembled nanostructures, crystallisation phenomena (ii) materials science, e.g., batteries, catalysts, hydrogen storage and motion, metal-organic frameworks, carbon capture, cement, tissue scaffolds, storage of nuclear waste (iii) biology, e.g., plant cell walls, protein complexes, membrane proteins, bone and biomineral structure Considering specific examples: understanding of intermolecular interactions will lead to better pharmaceutical formulations for enhanced drug delivery; knowledge of the underlying chemistry will enable better energy materials and catalysts to be produced; insight into the molecular basis of plant cell wall properties impacts on recalcitrance, which hinders the use of plant biomass for renewable energy by inhibiting the conversion into fermentable sugars. Industry has accessed the state-of-the-art solid-state NMR instrumentation either via either via paid-for industrial contract research or through industry support of PhD student users of the Facility, for example, the pharmaceutical (e.g., AstraZeneca and GlaxoSmithKline), oil/ fuel (e.g., Infineum and Sasol) and catalysis/ materials (e.g., BP, Johnson Matthey) industry. |
First Year Of Impact | 2011 |
Sector | Agriculture, Food and Drink,Chemicals,Energy,Healthcare,Manufacturing, including Industrial Biotechology,Pharmaceuticals and Medical Biotechnology |
Impact Types | Societal,Economic |