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Cryogenic 35GHz pulse ENDOR probehead accommodating large sample sizes: Performance and applications.

René Tschaggelar1, Besnik Kasumaj, Maria Grazia Santangelo

  • 1Laboratory of Physical Chemistry, ETH Zurich, Zürich CH-8093, Switzerland.

Journal of Magnetic Resonance (San Diego, Calif. : 1997)
|July 8, 2009
PubMed
Summary

A new cryogenic 35GHz pulse electron nuclear double resonance (ENDOR) probehead for large samples was constructed. This probehead enhances experimental efficiency and applicability for paramagnetic samples containing transition metal ions.

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Area of Science:

  • Physics
  • Chemistry
  • Spectroscopy

Background:

  • Electron Nuclear Double Resonance (ENDOR) is a powerful technique for studying paramagnetic species.
  • Cryogenic probeheads are essential for maintaining sample stability and improving signal-to-noise ratios at low temperatures.
  • Previous ENDOR probeheads often had limitations regarding sample size, restricting certain applications.

Purpose of the Study:

  • To present the construction and performance of a novel cryogenic 35GHz pulse ENDOR probehead.
  • To enable the study of larger sample volumes, thereby increasing sensitivity and applicability.
  • To investigate the electromagnetic field distributions within the probehead for optimized performance.

Main Methods:

  • Design and construction of a rectangular TE(102) cavity resonator.
  • Integration of a two-turn saddle coil for radio frequency (rf) B(2)-field generation.
  • Electromagnetic field calculations including all dielectric components, sample tube, and coupling elements.
  • Characterization using an rf power efficiency factor over a 2-180MHz frequency range.

Main Results:

  • Successful construction and characterization of the cryogenic 35GHz pulse ENDOR probehead.
  • Detailed analysis of microwave B(1)- and E(1)-field, and rf B(2)-field distributions.
  • Demonstration of the probehead's applicability and advantages for large sample sizes.
  • Validation using paramagnetic samples containing transition metal ions.

Conclusions:

  • The developed cryogenic 35GHz pulse ENDOR probehead is effective for large samples.
  • The design allows for efficient generation of the rf B(2)-field.
  • This advancement broadens the scope of ENDOR studies, particularly for transition metal ion-containing samples.