Abstract
This contribution presents a novel design of a double-resonance structure for high-field dynamic nuclear polarization operating at 95 GHz and 144 MHz, in which a miniaturized radiofrequency coil is integrated within a single-mode nonradiative dielectric resonator. After a detailed discussion of the design principles, the conversion factors of this system are determined by means of microwave and radiofrequency measurements. The obtained results, 1.68 mT/W1/2 for the microwave conversion factor and 0.8 mT/W1/2 for the radiofrequency conversion factor, represent the state-of-the-art among the double-resonance structures. Simultaneous electron paramagnetic resonance and liquid-state 1H nuclear magnetic resonance experiments are performed on samples of nitroxide radical 2,2,6,6-tetramethylpiperidine-1-oxyl dissolved in a mixture of water and dioxane. A maximum dynamic nuclear polarization enhancement of about −16 is obtained at a microwave power of 70 mW with a radical concentration of 10 mM in nanoliter-sized sample volumes. These results are discussed in view of further improvements and applications of the proposed double-resonance structure.
Similar content being viewed by others
References
A.W. Overhauser, Phys. Rev. 92, 411 (1953)
T.R. Carver, C.P. Slichter, Phys. Rev. 92, 212 (1953)
A. Abragam, The Principles of Nuclear Magnetism (Clarendon, Oxford, 1961)
A.V. Kessenikh, V.I. Lushchikov, A.A. Manenkov, Y.V. Taran, Sov. Phys. Solid State 5, 321 (1963)
A.V. Kessenikh, A.A. Manenkov, G.I. Pyatnitskii, Sov. Phys. Solid State 6, 641 (1964)
C.F. Hwang, D.A. Hill, Phys. Rev. Lett. 18, 110 (1967)
C.F. Hwang, D.A. Hill, Phys. Rev. Lett. 19, 1011 (1967)
D.S. Wollan, Phys. Rev. B 13, 3671 (1976)
R.A. Wind, M.J. Duijvestijn, C. van der Luat, A. Manenschijn, J. Vriend, Prog. Nucl. Magn. Reson. Spectrosc. 17, 33 (1985)
T. Maly, G.T. Debelouchina, V.S. Bajaj, K.N. Hu, C.G. Joo, M.L. Mak-Jurkauskas, J.R. Sirigiri, P.C.A. van der Wel, J. Herzfeld, R.J. Temkin, R.G. Griffin, J. Chem. Phys. 128, 052211 (2008)
K.H. Hausser, D. Stehlik, Adv. Magn. Reson. 3, 79 (1968)
G. Denninger, W. Stocklein, E. Dormann, M. Schwoerer, Mol. Cryst. Liq. Cryst. 120, 233–236 (1985)
K.N. Hu, H.H. Yu, T.M. Swager, R.G. Griffin, J. Am. Chem. Soc. 126, 10844–10845 (2004)
C. Song, K.N. Hu, C.G. Joo, T.M. Swager, R.G. Griffin, J. Am. Chem. Soc. 128, 11385–11390 (2006)
E.R. McCarney, B.D. Armstrong, M.D. Lingwood, S. Han, Proc. Natl. Acad. Sci. USA 104, 1754–1759 (2007)
B.D. Armstrong, S. Han, J. Am. Chem. Soc. 131, 4641–4647 (2009)
J.H. Ardenkjaer-Larsen, B. Fridlund, A. Gram, G. Hansson, L. Hansson, M.H. Lerche, R. Servin, M. Thaning, K. Golman, Proc. Natl. Acad. Sci. USA 100, 10158–10163 (2003)
Appl. Magn. Reson. 34 (2008)
L. Frydman, C. R. Chim. 9, 336–345 (2006)
Y. Shrot, L. Frydman, J. Magn. Reson. 195, 226–231 (2008)
Y. Shrot, L. Frydman, J. Chem. Phys. 128, 052209 (2008)
Y. Shrot, L. Frydman, J. Chem. Phys. 128, 164513 (2008)
L.R. Becerra, G.J. Gerfen, R.J. Temkin, D.J. Singel, R.G. Griffin, Phys. Rev. Lett. 71, 3561 (1993)
M.K. Hornstein, V.S. Bajaj, R.G. Griffin, K.E. Kreischer, I. Mastovsky, M.A. Shapiro, J.R. Sirigiri, IEEE Trans. Electron Devices 52, 798–807 (2005)
V.S. Bajaj, M.K. Hornstein, K.E. Kreischer, J.R. Sirigiri, P.P. Woskov, M.L. Mak-Jurkauskas, J. Herzfeld, R.J. Temkin, R.G. Griffin, J. Magn. Reson. 189, 251–279 (2007)
T. Idehara, T. Saito, I. Ogawa, S. Mitsudo, Y. Tatematsu, L. Agusu, H. Mori, S. Kobayashi, Appl. Magn. Reson. 34, 265–275 (2008)
M. Glyavin, V. Khizhnyak, A. Luchinin, T. Idehara, T. Saito, Int. J. Infrared Millimeter Waves 29, 641–648 (2008)
V. Weis, M. Bennati, M. Rosay, J.A. Bryant, R.G. Griffin, J. Magn. Reson. 140, 293–299 (1999)
C.P. Poole, Electron Spin Resonance: a Comprehensive Treatise on Experimental Techniques (Wiley, New York, 1983)
A.P.M. Kentgens, J. Bart, P.J.M. van Bentum, A. Brinkmann, E.R.H. Van Eck, J.G.E. Gardeniers, J.W.G. Janssen, P. Knijn, S. Vasa, M.H.W. Verkuijlen, J. Chem. Phys. 128, 052202 (2008)
D.J. Singel, H. Seidel, R.D. Kendrick, C.S. Yannoni, J. Magn. Reson. 81, 145–161 (1989)
R.A. Wind, R.A. Hall, A. Jurkiewicz, H. Lock, G.E. Maciel, J. Magn. Reson. A110, 33–37 (1994)
H. Cho, J. Baugh, C.A. Ryan, D.G. Cory, C. Ramanathan, J. Magn. Reson. 187, 242–250 (2007)
M. Bennati, C.T. Farrar, J.A. Bryant, S.J. Inati, V. Weis, G.J. Gerfen, P. Riggs-Gelasco, J. Stubbe, R.G. Griffin, J. Magn. Reson. 138, 232–243 (1999)
P. Hofer, G. Parigi, C. Luchinat, P. Carl, G. Guthausen, M. Reese, T. Carlomagno, C. Griesinger, M. Bennati, J. Am. Chem. Soc. 130, 3254 (2008)
J.S. Hyde, J. Chem. Phys. 43, 1806 (1965)
K.P. Dinse, K. Möbius, R. Biehl, Z. Naturforsch. 28a, 1069 (1973)
I.M. Brown, D.J. Sloop, Rev. Sci. Instrum. 41, 1774 (1970)
K. Gruber, J. Forrer, A. Schweiger, H.H. Gunthard, J. Phys. E Sci. Istrum. 7, 569–576 (1973)
V.P. Denysenkov, M.J. Prandolini, A. Krahn, M. Gafurov, B. Endeward, T.F. Prisner, Appl. Magn. Reson. 34, 289–299 (2008)
G. Annino, M. Cassettari, M. Martinelli, IEEE Trans. Microwave Theory Tech. 57, 775–783 (2009)
G. Annino, M. Fittipaldi, M. Martinelli, H. Moons, S. Van Doorslaer, E Goovaerts. J. Magn. Reson. 200, 29–37 (2009). doi:10.1016/j.jmr.2009.05.011
G. Annino, M. Cassettari, M. Martinelli, P.J.M. van Bentum, Appl. Magn. Reson. 24, 157–175 (2003)
G. Annino, M. Cassettari, M. Fittipaldi, M. Martinelli, J. Magn. Reson. 176, 37–46 (2005)
G. Annino, M. Cassettari, M. Martinelli, Rev. Sci. Instrum. 76, 084702 (2005)
G. Annino, M. Cassettari, M. Martinelli, Rev. Sci. Instrum. 76, 064702 (2005)
G. Annino, M. Cassettari, M. Martinelli, Appl. Magn. Reson. 26, 447–456 (2004)
J. Krupka, A. Milewski, J. Phys. E Sci. Instrum. 12, 391–396 (1979)
H. Seidel, Z. Phys. 165, 239 (1961)
I. Tkach, A. Baldansuren, E. Kalabukhova, S. Lukin, A. Sitnikov, A. Tsvir, M. Ischenko, Y. Rosentzweig, E. Roduner, Appl. Magn. Reson. 35, 95–112 (2008)
R.A. Wind, J.H. Ardenkjaer-Larsen, J. Magn. Reson. 141, 347–354 (1999)
A. Savitsky, A.A. Dubinskii, M. Plato, Y.A. Grishin, H. Zimmermann, K. Möbius, J. Phys. Chem. B 112, 9079–9090 (2008)
B.D. Armstrong, S. Han, J. Chem. Phys. 127, 104508 (2007)
M.J. Prandolini, V.P. Denysenkov, M. Gafurov, S. Lyubenova, B. Endeward, M. Bennati, T.F. Prisner, Appl. Magn. Reson. 34, 399–407 (2008)
Acknowledgments
We kindly acknowledge Nederlandse Organisatie voor Wetenschappelijk Onderzoek (NWO), the European Cooperation in Science and Technology (COST) action P15 “Advanced paramagnetic resonance methods in molecular biophysics”, and the Short-Term Mobility programme of the National Research Council (CNR) for the financial support.
Author information
Authors and Affiliations
Corresponding author
Rights and permissions
About this article
Cite this article
Annino, G., Villanueva-Garibay, J.A., van Bentum, P.J.M. et al. A High-Conversion-Factor, Double-Resonance Structure for High-Field Dynamic Nuclear Polarization. Appl Magn Reson 37, 851 (2010). https://doi.org/10.1007/s00723-009-0091-6
Received:
Revised:
Published:
DOI: https://doi.org/10.1007/s00723-009-0091-6