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Samoson

Senior Research Scientist

Ago Samoson, PhD

Phone  +372 5063036 , e-mail ago.samoson@gmail.com

Sample Spinning NMR

Magnetic and electric interactions of nuclear spins are in many cases observable as small changes of Zeeman transition frequency in a strong external magnetic field.  The nuclear spin interactions provide valuable data on local structure and dynamics of very broad range of materials.
    Relevant shifts in Zeeman transition, observed in Nuclear Magnetic Resonance (NMR) experiment, can be of the order of  a fraction of a Hertz to about several hundred  kHz. This frequency range can be attained also by periodic mechanical motion of macroscopical objects. Mechanical reorientation of the sample brings about change of direction of the strong magnetic field relative to e.g. internuclear space vector, giving us a powerful tool for manipulating the content of the spectral information.
    We investigate limits of various NMR techniques based on different fast sample spinning techniques.  State of the art probeheads permit rotation of the sample at speeds up to 70,000 Hz and acceleration up to 1,000,000 Hz/s for motion of sample around single axis, for simultaneous rotation about two axes speeds 10,000/2,000 Hz have been reached.
    The research presumes  very multidisciplinary approach, spanning from classical to quantum mechanics, high tensile strength technical ceramics, aerodynamics and tribology, electrodynamics and electronics, high precision machining and grinding, real time software and pneumatics, basic theory and scripting of nuclear spin choreography, all contribute to design and operation of a solid state NMR probehead.
    Our work is characterized by close cooperation with other research groups on development, test and application of new techniques for the study of  HTC and battery materials, zeolites, polymers and biological macromolecules, using order of magnitude different magnets, from 4.7 to 45 T.

Selected Publications: 

  1. Howes AP, Anupold T, Lemaitre V, Kukol A, Watts A, Samoson A, Smith
    ME, Dupree R (2006) 'Enhancing resolution and sensitivity of O-17
    solid-state NMR through combining double rotation, H-1 decoupling and
    satellite modulation for biomolecular applications ', Chemical Physics
    Letters, 421 (1-3), 42 - 46 (0009-2614) pdf
  2. Kentgens APM, van Eck ERH, Ajithkumar TG, Anupõld T, Past J, Reinhold A, Samoson A, New opportunities for double rotation NMR of half-integer quadrupolar nuclei
    JOURNAL OF MAGNETIC RESONANCE 178 (2): 212-219 FEB 2006 pdf
  3. Traer JW, Montoneri E, Samoson A, Past J, Tuherm T, Goward GR
    Unraveling the complex hydrogen bonding of a dual-functionality proton conductor using ultrafast magic angle spinning NMR
    CHEMISTRY OF MATERIALS 18 (20): 4747-4754 OCT 3 2006
  4. Wong A, Pike KJ, Jenkins R, Clarkson GJ, Anupõld T, Howes AP, Crout DHG, Samoson A, Dupree R, Smith ME, Experimental and theoretical O-17 NMR study of the influence of hydrogen-bonding on C=O and O-H oxygens in carboxylic solids
    JOURNAL OF PHYSICAL CHEMISTRY A 110 (5): 1824-1835 FEB 9 2006
  5. Wong A, Howes AP, Pike KJ, Lemaitre V, Watts A, Anupõld T, Past J, Samoson A, Dupree R, Smith ME, New limits for solid-state O-17 NMR spectroscopy: Complete resolution of multiple oxygen sites in a simple biomolecule
    JOURNAL OF THE AMERICAN CHEMICAL SOCIETY 128 (24): 7744-7745 JUN 21 2006
  6. Ago Samoson, Tiit Tuherm, Jaan Past, Andres Reinhold, Tiit Anupõld, Ivo Heinmaa, New Horizons for Magic-Angle Spinning NMR, Topics in Current Chemistry, 246: 15–31, 2004, Springer-Verlag Berlin Heidelberg, 2004 pdf
  7. Carravetta M., Y. Murata, M. Murata, I. Heinmaa, R. Stern, A. Tontcheva, A. Samoson, Y. Rubin, K. Komatsu, and M. Levitt, Solid-State NMR Spectroscopy of Molecular Hydrogen Trapped Inside an Open-Cage Fullerene, J. Am. Chem. Soc., 126, 4092-4093, 2004 pdf
  8. K. J. Pike, V. Lemaitre, A. Kukol, T. Anupõld, A. Samoson, A. P. Howes, A. Watts, M. E. Smith, and R. Dupree, Solid-State 17O NMR of Amino Acids, J. Phys. Chem. B, 108, 9256-9263, 2004  pdf
  9. Jennifer E. Readman, Clare P. Grey, Martine Ziliox, Lucy M. Bull and Ago Samoson, Comparison of the 17O NMR spectra of zeolites LTA and LSX, Solid State Nuclear Magnetic Resonance, 26, 153–159, 2004  pdf
  10. Thomas, P. A.; Baldwin, A.; Dupree, R.; Blaha, P.; Schwarz, K.; Samoson, A.; Gan, Z. H.; Structure-Property Relationships in the Nonlinear Optical Crystal KTiOPO4 Investigated Using NMR and ab Initio DFT Calculations, J. Phys. Chem. B., 108(14), 4324-4331, 2004
  11. A. Samoson, T. Tuherm and J. Past, Rotation sweep NMR, Chem. Phys. Lett., 365, 292-299, 2002  pdf
  12. A.Samoson, Extended Magic-Angle Spinning , in Encyclopedia of Nuclear Magnetic Resonance, Volume 9: Advances in NMR, John Wiley & Sons, Ltd, pp. 59–64, 2002  pdf
  13. A. Samoson, T. Tuherm and Z. Gan,  High-Field High-Speed MAS Resolution Enhancement in 1H NMR Spectroscopy of Solids, Solid State Nuclear Magnetic Resonance, 20, 130-136, 2001  pdf
  14. A.Samoson, T.Tuherm,and J.Past, Ramped-speed cross polarization MAS NMR, J. Magn. Reson, 149, 264-267, 2001  pdf   
  15. A.Samoson, T.Anupõld, Synchronized double rotation 2D NMR, Solid State Nuclear Magnetic Resonance, 15, 217-225, 2000  pdf
  16. T. Anupold, A. Reinhold, P. Sarv, A. Samoson, A comparision of double rotation and multi-quantum magic angle spinning spectra, Solid State Nuclear Magnetic Resonance, 13, 87-91, 1998  pdf
  17. A.Samoson, Two-Dimensional Isotropic NMR of Quadrupole Nuclei in Solids, J. Magn. Reson, A121, 209-211, 1996  pdf
  18. A.Samoson, J.Tegenfeldt, Optimizing magic-angle spinning sideband supression, Solid State Nuclear Magnetic Resonance, 4, 53-58, 1995  pdf
  19. A.Samoson, Multiquantum NMR of quadrupole nuclei with strong pulses, Chem. Phys. Lett., 247, 203-206, 1995   pdf
  20. Samoson A, Introduction to DOR NMR, Nuclear Magnetic Resonance in Modern Technology NATO ASI Series C: Mathematical and Physical Sciences- Vol 447, p
    525-546, Kluwer 1994 pdf
  21. A. Samoson, B. Q. Sun, and A. Pines, New angles in motional averaging, in Pulsed Magnetic Resonance: NMR, ESR, and  Optics, A recognition of  E. L. Hahn, (ed. D. M. S. Bagguley), Oxford Science Publications, Oxford, pp. 80 - 94, 1992  pdf
  22. A.Samoson and A.Pines, Double rotor for solid-state NMR, Rev. Sci. Instrum., 60(10), 3239-3241, 1989  pdf
  23. A.Samoson and E.Lippmaa, 2D nutation spectroscopy in solids,  J. Magn. Reson, 79(2), 255-268, 1988  pdf
  24. A.Samoson, E.Lippmaa and A.Pines, High resolution solid-state N.M.R. Averaging of second-order effects by means of a double-rotor, Molecular Physics, Vol. 65, No. 4, 1013-1018, 1988  pdf
  25. A.Samoson, Satellite transition high-resolution NMR of quadrupolar nuclei in powders, Chem. Phys. Lett., 119, 1, 29-32, 1985   pdf
  26. A.Samoson and E.Lippmaa, Excitation phenomena and line intensities in high-resolution NMR powder spectra of half-integer quadrupolar nuclei, Physical Review B, Condensed Matter, Vol. 28, Third Series, No. 11, 6567-6570, 1983  pdf
  27. A.Samoson, E.Kundla and E.Lippmaa, High resolution MAS-NMR of quadrupolar nuclei in powders, J. Magn. Reson, 49(2), 350-357, 1982  pdf

Scientific projects:

ETF4929 Dynamic MAS NMR
01.01.01-31.12.04

ETF5138 Development of techniques for large-scale biosynthesis of  13C/2H/15N labeled peptides and proteins. Studies of structural and dynamical aspects of peptide hormone action by NMR in solution and in condensed phase
01.01.02-31.12.05

 


Viimati muudetud: 29.07.2010 (Urmas Suursalu) KBFI 2009