Optimal sensitivity for 1H detected relayed DNP of organic solids at fast MAS
Copyright © 2024 The Authors. Published by Elsevier Inc. All rights reserved..
Dynamic nuclear polarization (DNP) combined with high magnetic fields and fast magic angle spinning (MAS) has opened up a new avenue for the application of exceptionally sensitive 1H NMR detection schemes to study protonated solids. Recently, it has been shown that DNP experiments at fast MAS rates lead to slower spin diffusion and hence reduced DNP enhancements for impregnated materials. However, DNP enhancements alone do not determine the overall sensitivity of a NMR experiment. Here we measure the overall sensitivity of one-dimensional 1H detected relayed DNP experiments as a function of the MAS rate in the 20-60 kHz regime using 0.7 mm diameter rotors at 21.2 T. Although faster MAS rates are detrimental for the DNP enhancement on the target material, due to slower spin diffusion, we find that with increasing spinning rates the gain in sensitivity due to 1H line-narrowing and the folding-in of sideband intensity compensates a large part of the loss of overall hyperpolarization. We find that sensitivity depends on the atomic site in the molecule, and is maximised at between 40 and 50 kHz MAS for the sample of L-histidine.HCl·H2O studied here. There is a 10-20 % difference in sensitivity between the optimum MAS rate and the fastest rate currently accessible (60 kHz).
| Medienart: |
E-Artikel |
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| Erscheinungsjahr: |
2024 |
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| Erschienen: |
2024 |
| Enthalten in: |
Zur Gesamtaufnahme - volume:360 |
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| Enthalten in: |
Journal of magnetic resonance (San Diego, Calif. : 1997) - 360(2024) vom: 30. März, Seite 107645 |
| Sprache: |
Englisch |
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| Beteiligte Personen: |
Badoni, Saumya [VerfasserIn] |
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| Links: |
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| Themen: |
Dynamic nuclear polarization |
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| Anmerkungen: |
Date Revised 21.03.2024 published: Print-Electronic Citation Status PubMed-not-MEDLINE |
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| doi: |
10.1016/j.jmr.2024.107645 |
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| funding: |
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| Förderinstitution / Projekttitel: |
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| PPN (Katalog-ID): |
NLM368914550 |
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| 520 | |a Copyright © 2024 The Authors. Published by Elsevier Inc. All rights reserved. | ||
| 520 | |a Dynamic nuclear polarization (DNP) combined with high magnetic fields and fast magic angle spinning (MAS) has opened up a new avenue for the application of exceptionally sensitive 1H NMR detection schemes to study protonated solids. Recently, it has been shown that DNP experiments at fast MAS rates lead to slower spin diffusion and hence reduced DNP enhancements for impregnated materials. However, DNP enhancements alone do not determine the overall sensitivity of a NMR experiment. Here we measure the overall sensitivity of one-dimensional 1H detected relayed DNP experiments as a function of the MAS rate in the 20-60 kHz regime using 0.7 mm diameter rotors at 21.2 T. Although faster MAS rates are detrimental for the DNP enhancement on the target material, due to slower spin diffusion, we find that with increasing spinning rates the gain in sensitivity due to 1H line-narrowing and the folding-in of sideband intensity compensates a large part of the loss of overall hyperpolarization. We find that sensitivity depends on the atomic site in the molecule, and is maximised at between 40 and 50 kHz MAS for the sample of L-histidine.HCl·H2O studied here. There is a 10-20 % difference in sensitivity between the optimum MAS rate and the fastest rate currently accessible (60 kHz) | ||
| 650 | 4 | |a Journal Article | |
| 650 | 4 | |a Dynamic nuclear polarization | |
| 650 | 4 | |a Fast magic angle spinning | |
| 650 | 4 | |a Relayed dynamic nuclear polarization | |
| 650 | 4 | |a Solid-state NMR | |
| 700 | 1 | |a Berruyer, Pierrick |e verfasserin |4 aut | |
| 700 | 1 | |a Emsley, Lyndon |e verfasserin |4 aut | |
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