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Cryogenic Sample Loading into a Magic Angle Spinning Nuclear Magnetic Resonance Spectrometer that Preserves Cellular Viability

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Interferometrically stable, enclosed, spinning sample cell for spectroscopic experiments on air-sensitive samples.

Dmitry Baranov¹, Robert J Hill², Jisu Ryu¹

¹Department of Chemistry and Biochemistry, University of Colorado Boulder, Boulder, Colorado 80309, USA.

The Review of Scientific Instruments

|February 3, 2017

Summary

This summary is machine-generated.

A novel spinning sample cell enables rapid, vibration-free exchange of air-sensitive samples for high-repetition-rate experiments. This technology overcomes challenges in maintaining sample equilibrium and integrity during experiments with high photon flux.

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Area of Science:

Physical Chemistry
Spectroscopy
Materials Science

Background:

High photon flux experiments require rapid sample exchange to maintain equilibrium.
Existing methods face challenges with air-sensitive and vibration-sensitive samples.
Achieving high repetition rates is crucial for many advanced experiments.

Purpose of the Study:

To develop a compact spinning sample cell for air and moisture-sensitive liquids and thin films.
To enable rapid and complete sample exchange at high repetition rates (100 kHz).
To ensure compatibility with vibration-sensitive experimental setups.

Main Methods:

A sealed enclosure maintaining an oxygen/water-free environment (1 ppm).
A reusable, chemically inert glass sandwich cell integrated with a hard disk drive motor.
Achieving tangential speeds of 7-12 m/s at approximately 70 Hz rotation.

Main Results:

Demonstrated an oxygen and water-free environment using sodium benzophenone ketyl radical.
Enabled complete sample exchange at 100 kHz repetition rates.
The spinning cell operates acoustically silently and is compatible with high-stability interferometers.

Conclusions:

The spinning sample cell effectively addresses limitations in sample exchange for demanding experimental conditions.
It facilitates high-repetition-rate studies on sensitive samples without compromising experimental stability.
The developed system supports advanced photochemistry and spectroscopy research.