Preprints
https://doi.org/10.5194/mr-2021-12
https://doi.org/10.5194/mr-2021-12

  02 Feb 2021

02 Feb 2021

Review status: a revised version of this preprint is currently under review for the journal MR.

A novel sample handling system for dissolution dynamic nuclear polarization experiments

Thomas Kress1, Kateryna Che2, Ludovica M. Epasto2, Fanny Kozak2, Gregory L. Olsen2, Albina Selimovic2, and Dennis Kurzbach2 Thomas Kress et al.
  • 1Department of Chemistry, University of Cambridge, Lensfield Road, Cambridge CB2 1EW, UK
  • 2University Vienna, Faculty of Chemistry, Institute of Biological Chemistry, Währinger Str. 38, Vienna, Austria

Abstract. We present a system for facilitated sample vitrification, melting, and transfer in dissolution dynamic nuclear polarization (DDNP) experiments. For 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 four 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.

Thomas Kress et al.

Status: final response (author comments only)

Comment types: AC – author | RC – referee | CC – community | EC – editor | CEC – chief editor | : Report abuse
  • RC1: 'Comment on mr-2021-12', Anonymous Referee #1, 22 Mar 2021
    • AC1: 'Reply on RC1', Dennis Kurzbach, 23 Apr 2021
  • RC2: 'Comment on mr-2021-12', Anonymous Referee #2, 28 Mar 2021
    • AC2: 'Reply on RC2', Dennis Kurzbach, 23 Apr 2021
  • RC3: 'Comment on mr-2021-12', Anonymous Referee #3, 19 Apr 2021
  • EC1: 'Comment on mr-2021-12', Gottfried Otting, 26 Apr 2021

Thomas Kress et al.

Thomas Kress et al.

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Short summary
We present a system for facilitated sample vitrification, melting, and transfer in dissolution dynamic nuclear polarization experiments. The system enables inserting a sample through an airlock in combination with a dedicated dissolution system that is inserted through the same airlock shortly before the melting event. The cryostat can thus be operated continuously at low temperatures and the melting process is rapid as no pressurization steps of the cryostat are necessary for dissolution.