Jump to ContentJump to Main Navigation
Show Summary Details
More options …

Open Physics

formerly Central European Journal of Physics

Editor-in-Chief: Seidel, Sally

Managing Editor: Lesna-Szreter, Paulina

IMPACT FACTOR 2017: 0.755
5-year IMPACT FACTOR: 0.820

CiteScore 2018: 1.01

SCImago Journal Rank (SJR) 2018: 0.237
Source Normalized Impact per Paper (SNIP) 2018: 0.541

ICV 2017: 162.45

Open Access
See all formats and pricing
More options …
Volume 2, Issue 1


Volume 13 (2015)

NMR study of heterogeneity in pyridine-N-oxide...HCl crystal

Vytautas Balevicius / Alexandar Gacesa / Janez Plavec
Published Online: 2004-03-01 | DOI: https://doi.org/10.2478/BF02476276


An origin of narrow 1H NMR signals in pyridine-N-oxide (PyO)...HCl crystal has been investigated by means of MAS, SPEDAS, NOESY and COSY techniques. Spectra of crystalline samples are compared with those of solid phase obtained from liquid PyO...HCl solutions (in acetonitile/H2O) after the heterogeneous phase separation. It has been concluded that partially resolved peaks in 1H NMR spectra of solids are related with heterogeneity of spin system and presence of different H-bond clusters of water molecules. NOESY spectra show no cross-peaks even at very long mixing time (500 ms). This indicates there is no exchange process between spins causing different peaks, and thus the corresponding molecular aggregates are captured in “islands of mobility8 without any channels sufficient for exchange. Appearance of MAS side bands as “pseudo8 cross-peaks in 2D NMR spectra using MAS/COSY technique is reported. In the case of accidental coincidence of spinning frequency (ωMAS) with spectral distances between some diagonal signals, intensive non-diagonal peaks are observed at the corresponding cross-positions. A misleading conclusion concerning spin coupling is easy to avoid using various ωMAS.

Keywords: NMR spectroscopy; phase transitions; hydrogen bonding; pyridine-N-oxide

Keywords: 82.56.-b; 64.70.-p; 33.15.Fm

  • [1] V. Balevicius, A. Marsalka, V. Sablinskas and L. Kimtys: “Liquid-like Motion of Molecules in the Solid Phases of Organic Crystals as Studied by Raman and NMR Spectroscopy.”, J. Mol. Struct., Vol. 219, (1990), pp. 123–130. http://dx.doi.org/10.1016/0022-2860(90)80043-JCrossrefGoogle Scholar

  • [2] G. Dossech, C. Fressigne and A.H. Fuchs: “Premelting in Orientattionally Disordered Molecular Crystals. A Re-appraisal.”, J. Phys. Chem. Solids, Vol. 53, (1992), pp. 203–209. http://dx.doi.org/10.1016/0022-3697(92)90029-DCrossrefGoogle Scholar

  • [3] L. Kimtys, V. Balevicius and D.W. Aksenes: “Molecular Diffusion and Premelting in Hydrogen Bonded Organic Solids.”, J. Mol. Struct., Vol. 381, (1996), pp. 193–197. http://dx.doi.org/10.1016/0022-2860(95)09156-4CrossrefGoogle Scholar

  • [4] D.W. Aksnes and L. Kimtys: “1H NMR Studies of Cyclohexane Confined in Mesoporous Solids: Melting Point Depression and Pore Size Distribution.”, Appl. Magn. Reson., Vol. 23, (2002), pp. 51–62. http://dx.doi.org/10.1007/BF03166183CrossrefGoogle Scholar

  • [5] D.W. Aksnes, L.G. Gjerdåker and L. Kimtys: “Characterization of mesoporous materials by1H NMR.” In: J. Fraissard and O. Lapin (Eds.): Magnetic Resonance in Colloid and Interface Science (NATO Sci. Ser. II, Vol. 76), Kluwer Acad. Publ., Dordrecht, (2002), pp. 485–490. Google Scholar

  • [6] M.H. Levitt: Spin dynamics, John Wiley & Sons Ltd., Chichester, 2001. Google Scholar

  • [7] S. Ding and Ch.A. McDowell: ‘High-Resolution Proton NMR Spectra in Solids by Single-Pulse Excitation’, J. Magn. Reson. Ser. A, Vol. 111, (1994), pp. 212–214. http://dx.doi.org/10.1006/jmra.1994.1250CrossrefGoogle Scholar

  • [8] S. Ding and Ch.A. McDowell: “High-Resolution NMR Spectra of Nuclear Spin Systems under Homogeneous Interactions in Solids Exhibiting Line Narrowing Induced by the Memory Effect”, J. Magn. Reson. Ser. A, Vol. 117, (1995), pp. 171–178. http://dx.doi.org/10.1006/jmra.1995.0760CrossrefGoogle Scholar

  • [9] A.M. Gil, E. Alberti, C. Parreira, B.J. Goodfellow and B. Ravkin: “A Fast MAS1H NMR Study of Amino Acids and Proteins”, J. Mol. Struct., Vol. 602-603 (2002), pp. 357–366. http://dx.doi.org/10.1016/S0022-2860(01)00682-2CrossrefGoogle Scholar

  • [10] S. Ding and Ch.A. McDowell: “Two-Dimensional Proton Correlation Spectroscopy in Solids”, J. Magn. Reson. Ser. A, Vol. 115 (1995), pp. 141–144. http://dx.doi.org/10.1006/jmra.1995.1160CrossrefGoogle Scholar

  • [11] L. Zheng, K.W. Fisbein, R.G. Griffin and J. Herzfeld: “Two-Dimensional Solid-State1H-NMR and Proton Exchange”, J. Am. Chem. Soc., Vol. 115, (1993), pp. 6254–6261. http://dx.doi.org/10.1021/ja00067a045CrossrefGoogle Scholar

  • [12] V. Balevicius, J. Tamuliene and D. Hadzi: (to be published). Google Scholar

  • [13] K. Nishikawa, Y. Kasahara and T. Ichioka: “Inhomogeneity of Mixing in Acetonitrile Aqueous Solution Studied by Small-Angle X-ray Scattering”, J. Phys. Chem. B, Vol. 106, (2002), pp. 693–700. http://dx.doi.org/10.1021/jp011964vCrossrefGoogle Scholar

  • [14] D. Pfeninning and D. Woermann: “Modification of the Transport Properties of a Membrane by Selective Solvation: Hyperfiltration of Acetonitrile/Water Mixtures”, J. Membrane Sci., Vol. 32, (1987), pp. 105–116. http://dx.doi.org/10.1016/S0376-7388(00)81578-1CrossrefGoogle Scholar

  • [15] T. Narayanan, A. Kumar, S. Venkatachalam, J. Jacob and B.V. Prafulla: “Exploration of a quadruple critical point in a quaternary liquid mixture.”, J. Chem. Phys., Vol. 102, (1995), pp. 9653–9658. http://dx.doi.org/10.1063/1.468784CrossrefGoogle Scholar

  • [16] G. Schneider: “Phasengleichgewichte in fluessungen Systemen bei hohen Drucken”, Ber. Bunsenges. Phys. Chem., Vol. 70, (1966), pp. 497–612. Google Scholar

  • [17] M. Nakahara and Ch. Wakal: “Monomeric and Cluster States of Water Molecules in Organic Solvent”, Chem. Lett., (1992), pp. 809–812. CrossrefGoogle Scholar

About the article

Published Online: 2004-03-01

Published in Print: 2004-03-01

Citation Information: Open Physics, Volume 2, Issue 1, Pages 120–131, ISSN (Online) 2391-5471, DOI: https://doi.org/10.2478/BF02476276.

Export Citation

© 2004 Versita Warsaw. This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 3.0 License. BY-NC-ND 3.0

Citing Articles

Here you can find all Crossref-listed publications in which this article is cited. If you would like to receive automatic email messages as soon as this article is cited in other publications, simply activate the “Citation Alert” on the top of this page.

Vytautas Balevicius, Kestutis Aidas, Jelena Tamuliene, and Hartmut Fuess
Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy, 2005, Volume 61, Number 5, Page 835

Comments (0)

Please log in or register to comment.
Log in