Proton dynamics in letovicite, (NH4)3H(SO4)2: A 1H and 14N NMR spectroscopic study

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Authors

  • Michael Fechtelkord
  • Astrid Engelhardt
  • Josef Christian Buhl
  • Lutz Schwalowsky
  • Ulrich Bismayer

Research Organisations

External Research Organisations

  • Universität Hamburg
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Details

Original languageEnglish
Pages (from-to)76-88
Number of pages13
JournalSolid State Nuclear Magnetic Resonance
Volume17
Issue number1-4
Publication statusE-pub ahead of print - 20 Mar 2002

Abstract

The improper ferroelastic phase letovicite (NH4)3H(SO4)2 has been studied by 1H MAS NMR as well as by static 14N NMR experiments in the temperature range of 296-425 K. The 1H MAS NMR resonance from ammonium protons can be well distinguished from that of acidic protons. A third resonance appears just below the phase transition temperature which is due to the acidic protons in the paraelastic phase. The lowering of the second moment M2 for the ammonium protons takes place in the same temperature range as the formation of domain boundaries, while the signals of the acidic protons suffer a line narrowing in the area of Tc. The static 14N NMR spectra confirm the temperature of the motional changes of the ammonium tetrahedra. Two-dimensional 1H NOESY spectra indicate a chemical exchange between ammonium protons and the acidic protons of the paraphase.

Keywords

    2D NOESY, N, H, Ferroelastic, MAS, Solid-state NMR, Superprotonic conductivity

ASJC Scopus subject areas

Cite this

Proton dynamics in letovicite, (NH4)3H(SO4)2: A 1H and 14N NMR spectroscopic study. / Fechtelkord, Michael; Engelhardt, Astrid; Buhl, Josef Christian et al.
In: Solid State Nuclear Magnetic Resonance, Vol. 17, No. 1-4, 20.03.2002, p. 76-88.

Research output: Contribution to journalArticleResearchpeer review

Fechtelkord, M, Engelhardt, A, Buhl, JC, Schwalowsky, L & Bismayer, U 2002, 'Proton dynamics in letovicite, (NH4)3H(SO4)2: A 1H and 14N NMR spectroscopic study', Solid State Nuclear Magnetic Resonance, vol. 17, no. 1-4, pp. 76-88. https://doi.org/10.1006/snmr.2000.0006
Fechtelkord, M., Engelhardt, A., Buhl, J. C., Schwalowsky, L., & Bismayer, U. (2002). Proton dynamics in letovicite, (NH4)3H(SO4)2: A 1H and 14N NMR spectroscopic study. Solid State Nuclear Magnetic Resonance, 17(1-4), 76-88. Advance online publication. https://doi.org/10.1006/snmr.2000.0006
Fechtelkord M, Engelhardt A, Buhl JC, Schwalowsky L, Bismayer U. Proton dynamics in letovicite, (NH4)3H(SO4)2: A 1H and 14N NMR spectroscopic study. Solid State Nuclear Magnetic Resonance. 2002 Mar 20;17(1-4):76-88. Epub 2002 Mar 20. doi: 10.1006/snmr.2000.0006
Fechtelkord, Michael ; Engelhardt, Astrid ; Buhl, Josef Christian et al. / Proton dynamics in letovicite, (NH4)3H(SO4)2 : A 1H and 14N NMR spectroscopic study. In: Solid State Nuclear Magnetic Resonance. 2002 ; Vol. 17, No. 1-4. pp. 76-88.
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abstract = "The improper ferroelastic phase letovicite (NH4)3H(SO4)2 has been studied by 1H MAS NMR as well as by static 14N NMR experiments in the temperature range of 296-425 K. The 1H MAS NMR resonance from ammonium protons can be well distinguished from that of acidic protons. A third resonance appears just below the phase transition temperature which is due to the acidic protons in the paraelastic phase. The lowering of the second moment M2 for the ammonium protons takes place in the same temperature range as the formation of domain boundaries, while the signals of the acidic protons suffer a line narrowing in the area of Tc. The static 14N NMR spectra confirm the temperature of the motional changes of the ammonium tetrahedra. Two-dimensional 1H NOESY spectra indicate a chemical exchange between ammonium protons and the acidic protons of the paraphase.",
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AU - Buhl, Josef Christian

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AU - Bismayer, Ulrich

N1 - Funding Information: The authors gratefully acknowledge fruitful discussions on proton dynamics with Ulrike Werner-Zwanziger of the University of Indiana, Department of Chemistry (Bloomington, IN), and Colin A. Fyfe, University of British Columbia (Vancouver, Canada). M. Fechtelkord thanks the Alexander von Humboldt foundation for a Feodor Lynen research fellowship.

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