A novel sample handling system for dissolution dynamic nuclear polarization experiments

We present a system for facilitated sample vitrification, melting, and transfer in dissolution dynamic nuclear polarization (DDNP) experiments. In DDNP, a sample is typically hyperpolarized at cryogenic temperatures before dissolution with hot solvent and transfer to a nuclear magnetic resonance (NM...

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Bibliographic Details
Published in:Magnetic Resonance : (Göttingen) 2021, Vol.2 (1), p.387-394
Main Authors: Kress, Thomas, Che, Kateryna, Epasto, Ludovica M, Kozak, Fanny, Negroni, Mattia, Olsen, Gregory L, Selimovic, Albina, Kurzbach, Dennis
Format: Article
Language:English
Subjects:
Blood vessels
Cryogenic temperature
Decay rate
Dissolution
Freezing
Heat
Hyperpolarization
Low temperature
Melting
NMR
Nuclear magnetic resonance
Polarization
Solvents
Vitrification
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Summary:We present a system for facilitated sample vitrification, melting, and transfer in dissolution dynamic nuclear polarization (DDNP) experiments. In DDNP, a sample is typically hyperpolarized at cryogenic temperatures before dissolution with hot solvent and transfer to a nuclear magnetic resonance (NMR) spectrometer for detection in the liquid state. The resulting signal enhancements can exceed 4 orders of magnitude. However, the sudden temperature jump from cryogenic temperatures close to 1 K to ambient conditions imposes a particular challenge. It is necessary to rapidly melt the sample to avoid a prohibitively fast decay of hyperpolarization. Here, we demonstrate a sample dissolution method that facilitates the temperature jump by eliminating the need to open the cryostat used to cool the sample. This is achieved by inserting the sample through an airlock in combination with a dedicated dissolution system that is inserted through the same airlock shortly before the melting event. The advantages are threefold: (1) the cryostat can be operated continuously at low temperatures. (2) The melting process is rapid as no pressurization steps of the cryostat are required. (3) Blockages of the dissolution system due to freezing of solvents during melting and transfer are minimized.
ISSN:2699-0016
2699-0016
DOI:10.5194/mr-2-387-2021