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research article

H-1 Detected Relayed Dynamic Nuclear Polarization

Berruyer, Pierrick  
•
Bertarello, Andrea  
•
Bjoergvinsdottir, Snaedis
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May 5, 2022
Journal Of Physical Chemistry C

Recently, it has been shown that methods based on the dynamics of 1 H nuclear hyperpolarization in magic angle spinning (MAS) NMR experiments can be used to determine mesoscale structures in complex materials. However, these methods suffer from low sensitivity, especially since they have so far only been feasible with indirect detection of 1 H polarization through dilute heteronuclei such as 13C or 29Si. Here we combine relayed-DNP (R-DNP) with fast MAS using 0.7 mm diameter rotors at 21.2 T. Fast MAS enables direct 1 H detection to follow hyperpolarization dynamics, leading to an acceleration in experiment times by a factor 16. Furthermore, we show that by varying the MAS rate, and consequently modulating the 1 H spin diffusion rate, we can record a series of independent R-DNP curves that can be analyzed jointly to provide an accurate determination of domain sizes. This is confirmed here with measurements on microcrystalline L-histidinemiddotHClmiddotH2O at MAS frequencies up to 60 kHz, where we determine a Weibull distribution of particle sizes centered on a radius of 440 +/- 20 nm with an order parameter of k = 2.2.

  • Details
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Type
research article
DOI
10.1021/acs.jpcc.2c01077
Web of Science ID

WOS:000814854000024

Author(s)
Berruyer, Pierrick  
Bertarello, Andrea  
Bjoergvinsdottir, Snaedis
Lelli, Moreno
Emsley, Lyndon  
Date Issued

2022-05-05

Published in
Journal Of Physical Chemistry C
Volume

126

Issue

17

Start page

7564

End page

7570

Subjects

Chemistry, Physical

•

Nanoscience & Nanotechnology

•

Materials Science, Multidisciplinary

•

Chemistry

•

Science & Technology - Other Topics

•

Materials Science

•

spin-diffusion

•

nmr-spectroscopy

•

hyperpolarization

•

sizes

Editorial or Peer reviewed

REVIEWED

Written at

EPFL

EPFL units
LRM  
FunderGrant Number

FNS

200020_178860

Available on Infoscience
July 4, 2022
Use this identifier to reference this record
https://infoscience.epfl.ch/handle/20.500.14299/188873
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