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research article

A spinning thermometer to monitor microwave heating and glass transitions in dynamic nuclear polarization

Miéville, Pascal  
•
Vitzthum, Veronika  
•
Caporini, Marc A.  
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2011
Magnetic Resonance in Chemistry

As previously demonstrated by Thurber and Tycko, the peak position of Br-79 in potassium bromide (KBr) allows one to determine the temperature of a spinning sample. We propose to adapt the original design by using a compact KBr tablet placed at the bottom of the magic angle spinning rotor, separated from the sample under investigation by a thin disk made of polytetrafluoroethylene (or 'Teflon'(R)). This design allows spinning the sample up to at least 16 kHz. The KBr tablet can remain in the rotor when changing the sample under investigation. Calibration in the range of 98 < T < 320 K has been carried out in a static rotor by inserting a platinum thermometer. The accuracy is better than +/- 0.9 K, even in the presence of microwave irradiation. Irradiation with 5W microwaves at 263 GHz leads to a small temperature increase of 3.6 +/- 1.4 K in either static or spinning samples. The dynamic nuclear polarization enhancement decreases with increasing temperature, in particular when a frozen glassy sample undergoes a glass transition. Copyright (C) 2011 John Wiley & Sons, Ltd.

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Type
research article
DOI
10.1002/mrc.2811
Web of Science ID

WOS:000296609600001

Author(s)
Miéville, Pascal  
Vitzthum, Veronika  
Caporini, Marc A.  
Jannin, Sami  
Gerber-Lemaire, Sandrine  
Bodenhausen, Geoffrey  
Date Issued

2011

Publisher

Wiley-Blackwell

Published in
Magnetic Resonance in Chemistry
Volume

49

Issue

11

Start page

689

End page

692

Subjects

dynamic nuclear polarization

•

magic angle spinning (MAS)

•

MAS thermometry

•

potassium bromide (KBr)

•

glass transition

•

Solid-State

•

Aqueous-Solutions

•

Chemical-Shift

•

Dependence

•

Methanol

•

Glycol

•

Nmr

•

Kbr

Editorial or Peer reviewed

REVIEWED

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Available on Infoscience
September 15, 2011
Use this identifier to reference this record
https://infoscience.epfl.ch/handle/20.500.14299/70956
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