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Influence of F content on the composition of Al-rich synthetic phlogopite: Part I. New information on structure and phase-formation from 29Si, 1H, and 19F MAS NMR spectroscopies

  • Michael Fechtelkord EMAIL logo , Harald Behrens , François Holtz , Colin A. Fyfe , Lee A. Groat and Mati Raudsepp
Published/Copyright: March 31, 2015
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American Mineralogist
From the journal American Mineralogist Volume 88 Issue 1

Abstract

The influence of F content on the formation and stability of Al-rich phlogopite has been investigated. Samples with varying OH/F-ratios and nominal gel compositions of K(Mg3-xAlx)(Al1+xSi3-xO10)(OH)y (F)2-y (0.0 < x < 0.8 and 0.5 < y < 1.8) were studied using 29Si, 1H, and 19F MAS NMR spec­troscopies, powder X-ray diffraction, electron-probe microanalysis, and scanning electron mi­croscopy. The synthetic phlogopites were synthesized from sol-gels in cold-seal pressure vessels at 1073 K, 2 kbar. The main phase (phlogopite) and three other impurity phases [corundum (α-Al2O3), kalsilite (KAlSiO4), and potassium aluminum hexafluoride (K3AlF6-0.5H20)] were clearly identi­fied by powder X-ray diffraction and electron-probe microanalysis. For phlogopite, the unit-cell parameters a0 and b0 decrease whereas C0 increases with increasing Al-content (x). The average crystal size of phlogopite is about 1-2 pm. The 29Si MAS NMR spectra show up to four resonances at approximately -91, -87, -83, and -80 ppm, which can be assigned as Q3(n Al) signals with n = 0 - 3. The ideal Si/ivAl ratio calculated from the initial composition is always lower than that derived experimentally. Hydroxyl-rich compositions indicate an increased Al-content in the tetrahedral sheets, suggesting a stabilizing effect on the formation of Al-rich phlogopite. These conclusions are sup­ported by 1H and 19F MAS NMR spectra. The 1H MAS NMR spectra show a water signal at 4.7 ppm, a signal due to Mg2AlOH at 1.8 ppm, and a signal due to Mg3OH at 0.7 ppm. The 19F MAS NMR spectra exhibit a signal for Mg2AlF at -150 ppm, one due to AlF6 (K3AlF6-0.5H20) at -157 ppm, and one for Mg3F at -174 ppm. Comparison of the 1H and 19F MAS NMR spectra for different Al- and F- contents reveals a non-statistical distribution of F- and OH-groups at the crystallographic sites in the octahedral sheets where F prefers sites coordinated by three Mg, and OH sites with Al in the next- nearest coordination sphere.

Received: 2001-7-24
Accepted: 2002-8-22
Published Online: 2015-3-31
Published in Print: 2003-1-1

© 2015 by Walter de Gruyter Berlin/Boston

Articles in the same Issue

  1. A molecular dynamics study of the behavior of sodium in low albite
  2. Observation and interpretation of paramagnetic defects in Brazilian and Central African carbonados
  3. Dissolution of gibbsite: Direct observations using fluid cell atomic force microscopy
  4. Polytypes and higher-order structures of antigorite: A TEM study
  5. An infrared spectroscopic study of the basic copper phosphate minerals: Cornetite, libethenite, and pseudomalachite
  6. Influence of F content on the composition of Al-rich synthetic phlogopite: Part I. New information on structure and phase-formation from 29Si, 1H, and 19F MAS NMR spectroscopies
  7. NMR evidence for formation of octahedral and tetrahedral Al and repolymerization of the Si network during dissolution of aluminosilicate glass and crystal
  8. Thermodynamic properties of hercynite (FeAl2O4) based on adiabatic calorimetry at low temperatures
  9. The formation of Sr silicates at low temperature and the solubility product of tobermorite-like Sr5Si6O16(OH)2 .5H2O
  10. Thermal equation of state of omphacite
  11. The effect of thermal decarbonation on stable isotope compositions of carbonates
  12. Synthetic MgAl2O4 (spinel) at high-pressure conditions (0.0001–30 GPa): A synchrotron X-ray powder diffraction study
  13. The stability of antigorite in the systems MgO-SiO2-H2O (MSH) and MgO-Al2O3-SiO2-H2O (MASH): The effects of Al3+ substitution on high-pressure stability
  14. The fusion curve of albite revisited and the compressibility of NaAlSi3O8 liquid with pressure
  15. Correction of secondary X-ray fluorescence near grain boundaries in electron microprobe analysis: Application to thermobarometry of spinel lherzolites
  16. An overgrowth model to explain multiple, dispersed high-Mn regions in the cores of garnet porphyroblasts
  17. Synchrotron X-ray diffraction study of the structure and dehydration behavior of todorokite
  18. Retrograde mineral reactions in saline fluid inclusions: The transformation ferropyrosmalite ↔ clinopyroxene
  19. The effect of ionizing radiation on uranophane
  20. Hydration, expansion, structure, and dynamics of layered double hydroxides
  21. Relict edenite in a garnet lherzolite from the Chinese Su-Lu UHP metamorphic terrane: Implications for metamorphic history
  22. Norrishite, K(Mn23+Li)Si4O10(O)2, an oxymica associated with sugilite from the Wessels Mine, South Africa: Crystal chemistry and 40Ar-39Ar dating
  23. The amblygonite (LiAlPO4F)-montebrasite (LiAlPO4OH) solid solution: A combined powder and single-crystal neutron diffraction and solid-state 6Li MAS, CP MAS, and REDOR NMR study
  24. An X-ray Rietveld, infrared, and Mössbauer spectral study of the NaMn(Fe1–xInx)2(PO4)3 alluaudite-type solid solution
  25. Gatelite-(Ce), a new REE-bearing mineral from Trimouns, French Pyrenees: Crystal structure and polysomatic relationships with epidote and törnebohmite-(Ce)
  26. Hydroxyl in clinopyroxene from the deep subducted crust: Evidence for H2O transport into the mantle
  27. A model for the structure of the hydrated aluminum phosphate, kingite determined by ab initio powder diffraction methods
  28. The crystal structure of synthetic autunite, Ca[(UO2)(PO4)]2(H2O)11
https://doi.org/10.2138/am-2003-0106

Articles in the same Issue

  1. A molecular dynamics study of the behavior of sodium in low albite
  2. Observation and interpretation of paramagnetic defects in Brazilian and Central African carbonados
  3. Dissolution of gibbsite: Direct observations using fluid cell atomic force microscopy
  4. Polytypes and higher-order structures of antigorite: A TEM study
  5. An infrared spectroscopic study of the basic copper phosphate minerals: Cornetite, libethenite, and pseudomalachite
  6. Influence of F content on the composition of Al-rich synthetic phlogopite: Part I. New information on structure and phase-formation from 29Si, 1H, and 19F MAS NMR spectroscopies
  7. NMR evidence for formation of octahedral and tetrahedral Al and repolymerization of the Si network during dissolution of aluminosilicate glass and crystal
  8. Thermodynamic properties of hercynite (FeAl2O4) based on adiabatic calorimetry at low temperatures
  9. The formation of Sr silicates at low temperature and the solubility product of tobermorite-like Sr5Si6O16(OH)2 .5H2O
  10. Thermal equation of state of omphacite
  11. The effect of thermal decarbonation on stable isotope compositions of carbonates
  12. Synthetic MgAl2O4 (spinel) at high-pressure conditions (0.0001–30 GPa): A synchrotron X-ray powder diffraction study
  13. The stability of antigorite in the systems MgO-SiO2-H2O (MSH) and MgO-Al2O3-SiO2-H2O (MASH): The effects of Al3+ substitution on high-pressure stability
  14. The fusion curve of albite revisited and the compressibility of NaAlSi3O8 liquid with pressure
  15. Correction of secondary X-ray fluorescence near grain boundaries in electron microprobe analysis: Application to thermobarometry of spinel lherzolites
  16. An overgrowth model to explain multiple, dispersed high-Mn regions in the cores of garnet porphyroblasts
  17. Synchrotron X-ray diffraction study of the structure and dehydration behavior of todorokite
  18. Retrograde mineral reactions in saline fluid inclusions: The transformation ferropyrosmalite ↔ clinopyroxene
  19. The effect of ionizing radiation on uranophane
  20. Hydration, expansion, structure, and dynamics of layered double hydroxides
  21. Relict edenite in a garnet lherzolite from the Chinese Su-Lu UHP metamorphic terrane: Implications for metamorphic history
  22. Norrishite, K(Mn23+Li)Si4O10(O)2, an oxymica associated with sugilite from the Wessels Mine, South Africa: Crystal chemistry and 40Ar-39Ar dating
  23. The amblygonite (LiAlPO4F)-montebrasite (LiAlPO4OH) solid solution: A combined powder and single-crystal neutron diffraction and solid-state 6Li MAS, CP MAS, and REDOR NMR study
  24. An X-ray Rietveld, infrared, and Mössbauer spectral study of the NaMn(Fe1–xInx)2(PO4)3 alluaudite-type solid solution
  25. Gatelite-(Ce), a new REE-bearing mineral from Trimouns, French Pyrenees: Crystal structure and polysomatic relationships with epidote and törnebohmite-(Ce)
  26. Hydroxyl in clinopyroxene from the deep subducted crust: Evidence for H2O transport into the mantle
  27. A model for the structure of the hydrated aluminum phosphate, kingite determined by ab initio powder diffraction methods
  28. The crystal structure of synthetic autunite, Ca[(UO2)(PO4)]2(H2O)11
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