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High resolution solid-state NMR on the desktop.
Xu, Ke; Aldudak, Fettah; Pecher, Oliver; Braun, Marco; Neuberger, Andreas; Foysi, Holger; Schmedt Auf der Günne, Jörn.
Afiliación
  • Xu K; University of Siegen, Faculty IV: School of Science and Technology, Department of Chemistry and Biology, Inorganic Materials Chemistry, Adolf-Reichwein-Str. 2, 57076, Siegen, Germany.
  • Aldudak F; University of Siegen, Faculty IV: School of Science and Technology, Department of Mechanical Engineering, Institute of Fluid and Thermodynamics, Paul-Bonatz-Str. 9-11, 57078, Siegen, Germany.
  • Pecher O; NMR Service GmbH, Blumenstr. 70 Haus 3, 99092, Erfurt, Germany.
  • Braun M; NMR Service GmbH, Blumenstr. 70 Haus 3, 99092, Erfurt, Germany.
  • Neuberger A; University of Siegen, Faculty IV: School of Science and Technology, Department of Chemistry and Biology, Inorganic Materials Chemistry, Adolf-Reichwein-Str. 2, 57076, Siegen, Germany.
  • Foysi H; University of Siegen, Faculty IV: School of Science and Technology, Department of Mechanical Engineering, Institute of Fluid and Thermodynamics, Paul-Bonatz-Str. 9-11, 57078, Siegen, Germany.
  • Schmedt Auf der Günne J; University of Siegen, Faculty IV: School of Science and Technology, Department of Chemistry and Biology, Inorganic Materials Chemistry, Adolf-Reichwein-Str. 2, 57076, Siegen, Germany. Electronic address: gunnej@chemie.uni-siegen.de.
Solid State Nucl Magn Reson ; 126: 101884, 2023 Aug.
Article en En | MEDLINE | ID: mdl-37419044
High-resolution low-field nuclear magnetic resonance (NMR) spectroscopy has found wide application for characterization of liquid compounds because of the low maintenance cost of modern permanent magnets. Solid-state NMR so far is limited to low-resolution measurements of static powders, because of the limited space available in this type of magnet. Magic-angle sample spinning and low-magnetic fields are an attractive combination to achieve high spectral resolution especially for paramagnetic solids. Here we show that magic angle spinning modules can be miniaturized using 3D printing techniques so that high-resolution solid-state NMR in permanent magnets becomes possible. The suggested conical rotor design was developed using finite element calculations and provides sample spinning frequencies higher than 20 kHz. The setup was tested on various diamagnetic and paramagnetic compounds including paramagnetic battery materials. The only comparable experiments in low-cost magnets known so far, had been done in the early times of magic angle spinning using electromagnets at much lower sample spinning frequency. Our results demonstrate that high-resolution low-field magic-angle-spinning NMR does not require expensive superconducting magnets and that high-resolution solid-state NMR spectra of paramagnetic compounds are feasible. Generally, this could introduce low-field solid-state NMR for abundant nuclei standard as a routine analytical tool.
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Texto completo: 1 Bases de datos: MEDLINE Idioma: En Revista: Solid State Nucl Magn Reson Asunto de la revista: DIAGNOSTICO POR IMAGEM / MEDICINA NUCLEAR Año: 2023 Tipo del documento: Article País de afiliación: Alemania

Texto completo: 1 Bases de datos: MEDLINE Idioma: En Revista: Solid State Nucl Magn Reson Asunto de la revista: DIAGNOSTICO POR IMAGEM / MEDICINA NUCLEAR Año: 2023 Tipo del documento: Article País de afiliación: Alemania