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High-Temperature and High-Pressure In situ Magic Angle Spinning Nuclear Magnetic Resonance Spectroscopy
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Diamond rotors for high magic angle spinning frequencies.

Lauren Schaffer1, David Preiss2, Ravi Shankar Palani1

  • 1Department of Chemistry and Francis Bitter Magnet Laboratory, Massachusetts Institute of Technology, Cambridge, MA 02139, United States.

Journal of Magnetic Resonance (San Diego, Calif. : 1997)
|July 8, 2025
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Summary

New diamond rotors for Magic Angle Spinning (MAS) nuclear magnetic resonance (NMR) spectroscopy enable higher spinning frequencies. These improved rotors overcome limitations of traditional zirconia rotors, enhancing spectral resolution for biological and material science applications.

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Area of Science:

  • Solid-state Nuclear Magnetic Resonance (NMR) Spectroscopy
  • Materials Science
  • Biophysics

Background:

  • Magic Angle Spinning (MAS) NMR spectroscopy's resolution is limited by rotor spinning frequencies.
  • Traditional yttria-stabilized zirconia (YSZ) rotors have mechanical constraints limiting spinning frequencies to ~110 kHz.
  • Higher frequencies (>300 kHz) are theoretically required for resolution comparable to solution NMR.

Purpose of the Study:

  • To develop advanced diamond rotors for MAS NMR to achieve higher spinning frequencies.
  • To improve rotor fabrication techniques for enhanced concentricity and spinning stability.
  • To evaluate diamond rotor performance and usability for biological and material science applications.

Main Methods:

  • Fabrication of diamond rotors using high-precision lathe and laser machining.
  • Testing rotor compatibility with Bruker MAS 3 spinning systems.
  • Evaluation of chemical vapor deposition (CVD) versus high-pressure high-temperature (HPHT) diamond materials.
  • 3D-printed tools for efficient rotor repacking.
  • Spin stability tests and multidimensional NMR of Aβ1-40.

Main Results:

  • Developed diamond rotors with improved concentricity and spinning stability.
  • Diamond rotors demonstrated compatibility and performance comparable to or exceeding commercial rotors.
  • HPHT diamond material was found to be preferable over CVD diamond.
  • Demonstrated robustness and usability through extended spin tests and NMR spectra.

Conclusions:

  • Advanced diamond rotor fabrication significantly enhances MAS NMR capabilities.
  • These rotors enable higher spinning frequencies, crucial for improved spectral resolution.
  • The developed technology paves the way for future advancements in MAS NMR for diverse scientific fields.