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Saturation recovery EPR and ELDOR at W-band for spin labels. J Magn Reson 2008 Aug;193(2):297-304

Date

06/13/2008

Pubmed ID

18547848

Pubmed Central ID

PMC2561891

DOI

10.1016/j.jmr.2008.05.008

Scopus ID

2-s2.0-47549115786   38 Citations

Abstract

A reference arm W-band (94 GHz) microwave bridge with two sample-irradiation arms for saturation recovery (SR) EPR and ELDOR experiments is described. Frequencies in each arm are derived from 2 GHz synthesizers that have a common time-base and are translated to 94 GHz in steps of 33 and 59 GHz. Intended applications are to nitroxide radical spin labels and spin probes in the liquid phase. An enabling technology is the use of a W-band loop-gap resonator (LGR) [J.W. Sidabras, R.R. Mett, W. Froncisz, T.G. Camenisch, J.R. Anderson, J.S. Hyde, Multipurpose EPR loop-gap resonator and cylindrical TE(011) cavity for aqueous samples at 94 GHz, Rev. Sci. Instrum. 78 (2007) 034701]. The high efficiency parameter (8.2 GW(-1/2) with sample) permits the saturating pump pulse level to be just 5 mW or less. Applications of SR EPR and ELDOR to the hydrophilic spin labels 3-carbamoyl-2,2,5,5-tetra-methyl-3-pyrroline-1-yloxyl (CTPO) and 2,2,6,6,-tetramethyl-4-piperidone-1-oxyl (TEMPONE) are described in detail. In the SR ELDOR experiment, nitrogen nuclear relaxation as well as Heisenberg exchange transfer saturation from pumped to observed hyperfine transitions. SR ELDOR was found to be an essential method for measurements of saturation transfer rates for small molecules such as TEMPONE. Free induction decay (FID) signals for small nitroxides at W-band are also reported. Results are compared with multifrequency measurements of T(1e) previously reported for these molecules in the range of 2-35 GHz [J.S. Hyde, J.-J. Yin, W.K. Subczynski, T.G. Camenisch, J.J. Ratke, W. Froncisz, Spin label EPR T(1) values using saturation recovery from 2 to 35 GHz. J. Phys. Chem. B 108 (2004) 9524-9529]. The values of T(1e) decrease at 94 GHz relative to values at 35 GHz.

Author List

Froncisz W, Camenisch TG, Ratke JJ, Anderson JR, Subczynski WK, Strangeway RA, Sidabras JW, Hyde JS

Authors

Jason W. Sidabras PhD Assistant Professor in the Biophysics department at Medical College of Wisconsin
Witold K. Subczynski PhD Professor in the Biophysics department at Medical College of Wisconsin




MESH terms used to index this publication - Major topics in bold

Electromagnetic Phenomena
Electron Spin Resonance Spectroscopy
Equipment Design
Equipment Failure Analysis
Microwaves
Spin Labels