A nuclear magnetic resonance spectrometer concept for hermetically sealed magic angle spinning investigations on highly toxic, radiotoxic, or air sensitive materials

Martel, L. and Somers, J. and Berkmann, C. and Koepp, F. and Rothermel, A. and Pauvert, O. and Selfslag, C. and Farnan, I. (2013) A nuclear magnetic resonance spectrometer concept for hermetically sealed magic angle spinning investigations on highly toxic, radiotoxic, or air sensitive materials. Review of Scientific Instruments, 84 (5). 055112-055112. ISSN 0034-6748, ESSN: 1089-7623 DOI 10.1063/1.4805017

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Official URL: http://rsi.aip.org/resource/1/rsinak/v84/i5/p05511...

Abstract

A concept to integrate a commercial high-resolution, magic angle spinning nuclear magnetic resonance (MAS-NMR) probe capable of very rapid rotation rates (70 kHz) in a hermetically sealed enclosure for the study of highly radiotoxic materials has been developed and successfully demonstrated. The concept centres on a conventional wide bore (89 mm) solid-state NMR magnet operating with industry standard 54 mm diameter probes designed for narrow bore magnets. Rotor insertion and probe tuning take place within a hermetically enclosed glovebox, which extends into the bore of the magnet, in the space between the probe and the magnet shim system. Oxygen-17 MAS-NMR measurements demonstrate the possibility of obtaining high quality spectra from small sample masses (∼10 mg) of highly radiotoxic material and the need for high spinning speeds to improve the spectral resolution when working with actinides. The large paramagnetic susceptibility arising from actinide paramagnetism in (Th1−xUx)O2 solid solutions gives rise to extensive spinning sidebands and poor resolution at 15 kHz, which is dramatically improved at 55 kHz. The first 17O MAS-NMR measurements on NpO2+x samples spinning at 55 kHz are also reported. The glovebox approach developed here for radiotoxic materials can be easily adapted to work with other hazardous or even air sensitive materials.

Item Type: Article
Additional Information: Review of Scientific Instruments is published by the American Institute of Physics. Copyright © 2013 American Institute of Physics. All rights reserved.This article may be downloaded for personal use only. Any other use requires prior permission of the author and the American Institute of Physics.
Uncontrolled Keywords: 2013AREP; IA66,
Subjects: 99 - Other
Divisions: 99 - Other
Journal or Publication Title: Review of Scientific Instruments
Volume: 84
Page Range: 055112-055112
Identification Number: 10.1063/1.4805017
Depositing User: Sarah Humbert
Date Deposited: 07 Jul 2013 00:29
Last Modified: 08 Aug 2013 12:14
URI: http://eprints.esc.cam.ac.uk/id/eprint/2819

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