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15N NMR study of nitrate ion structure and dynamics in hydrotalcite-like compounds

  • Xiaoqiang Hou EMAIL logo , R. James Kirkpatrick , Ping Yu , Duane Moore and Yeongkyoo Kim
Published/Copyright: March 25, 2015
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American Mineralogist
From the journal American Mineralogist Volume 85 Issue 1

Abstract

We report here the first nuclear magnetic resonance (NMR) spectroscopic study of the dynamical and structural behavior of nitrate on the surface and in the interlayer of hydrotalcite-like compounds (15NO3--HT). Spectroscopically resolvable surface-absorbed and interlayer NO3 - have dramatically different dynamical characteristics. The interlayer nitrate shows a well defined, temperature independent uniaxial chemical shift anisotropy (CSA) powder pattern. It is rigidly held or perhaps undergoes rotation about its threefold axis at all temperatures between -100 °C and +80 °C and relative humidities (R.H.) from 0 to 100% at room temperature. For surface nitrate, however, the dynamical behavior depends substantially on temperature and relative humidity. Analysis of the temperature and R.H. dependences of the peak width yields reorientational frequencies which increase from essentially 0 at -100 °C to 2.6 × 105 Hz at 60 °C and an activation energy of 12.6 kJ/mol. For example, for samples at R.H. = 33%, the surface nitrate is isotropically mobile at frequencies greater than 105 Hz at room temperature, but it becomes rigid or only rotates on its threefold axis at -100 °C. For dry samples and samples heated at 200 °C (R.H. near 0%), the surface nitrate is not isotropically averaged at room temperature. In contrast to our previous results for 35Cl--containing hydrotalcite (35Cl--HT), no NMR detectable structural phase transition is observed for 15NO-3-HT. The mobility of interlayer nitrate in HT is intermediate between that of carbonate and chloride.

Received: 1999-4-12
Accepted: 1999-8-5
Published Online: 2015-3-25
Published in Print: 2000-1-1

© 2015 by Walter de Gruyter Berlin/Boston

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https://doi.org/10.2138/am-2000-0116

Articles in the same Issue

  1. Eclogite-facies relics and inferred ultrahigh-pressure metamorphism in the North Dabie Complex, central-eastern China
  2. Application of INVEQ to the geothermobarometry of metamorphic rocks near a kyanite-sillimanite isograd, Mica Creek, British Columbia
  3. Microstructural characterization of metamorphic magnetite crystals with implications for oxygen isotope distribution
  4. Coexisting monazite and allanite in peraluminous granitoids of the TribečMountains, Western Carpathians
  5. Effect of alkalis, phosphorus, and water on the surface tension of haplogranite melt
  6. Direct observation of immiscibility in pyrope-almandine-grossular garnet
  7. On the cluster analysis of grains and crystals in rocks
  8. Experimental approach to constrain second critical end points in fluid/silicate systems: Near-solidus fluids and melts in the system albite-H2O
  9. Estimation and testing of standard molar thermodynamic properties of tourmaline end-members using data of natural samples
  10. An investigation of matrix effects in the analysis of fluorine in humite-group minerals by EMPA, SIMS, and SREF
  11. New data on the crystal-chemistry of fluoborite by means of SREF, SIMS, and EMP analysis
  12. Effect of aluminum on Ti-coordination in silicate glasses: A XANES study
  13. XAFS study of Cu model compounds and Cu2+ sorption products on amorphous SiO2, γ-Al2O3, and anatase
  14. Oxidation-reduction mechanism of iron in dioctahedral smectites: I. Crystal chemistry of oxidized reference nontronites
  15. Oxidation-reduction mechanism of iron in dioctahedral smectites: II. Crystal chemistry of reduced Garfield nontronite
  16. 15N NMR study of nitrate ion structure and dynamics in hydrotalcite-like compounds
  17. 29Si and 27Al MAS-NMR spectroscopy of b-eucryptite (LiAlSiO4): The enthalpy of Si,Al ordering
  18. The nuclear and magnetic structure of “white rust”—Fe(OH0.86D0.14)2
  19. In-situ study of the R3̅ to R3̅c phase transition in the ilmenite-hematite solid solution using time-of-flight neutron powder diffraction
  20. In situ X-ray diffraction investigation of lawsonite and zoisite at high pressures and temperatures
  21. A shell model for the simulation of rhombohedral carbonate minerals and their point defects
  22. Optical properties of natural and cation-exchanged heulandite group zeolites
  23. The crystal structure of gearksutite, CaAlF4(OH)· H2O
  24. A new anhydrous amphibole from the Eifel region, Germany: Description and crystal structure of obertiite, NaNa2(Mg3Fe3+Ti4+)Si8O22O2
  25. Kinoshitalite, Ba(Mg)3(Al2Si2)O10(OH,F)2, a brittle mica from a manganese deposit in Oman: Paragenesis and crystal chemistry
  26. The crystal structure of parisite-(Ce), Ce2CaF2(CO3)3
  27. High-pressure synthesis of Na2Mg6Si6O18(OH)2—a new hydrous silicate phase isostructural with aenigmatite
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