A novel sample handling system for dissolution dynamic nuclear polarization experiments
Magnetic resonance(2021)
摘要
Abstract. 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.
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