Synthesis, X-ray diffraction and MAS NMR characteristics of nitrate cancrinite Na7.6[AlSiO4]6(NO3)1.6(H2O)2

Research output: Contribution to journalArticleResearchpeer review

Authors

  • Josef Christian Buhl
  • Frank Stief
  • Michael Fechtelkord
  • Thorsten M. Gesing
  • Uwe Taphorn
  • Claudia Taake

Research Organisations

External Research Organisations

  • University of Münster
View graph of relations

Details

Original languageEnglish
Pages (from-to)93-102
Number of pages10
JournalJournal of alloys and compounds
Volume305
Issue number1-2
Early online date10 May 2000
Publication statusPublished - 6 Jun 2000

Abstract

Investigations on the hydrothermal formation and the crystal structure of nitrate cancrinite have been carried out in the system Na2O-xSiO2-Al2O3-NaNO3-H2O, 1<x<6. Various starting materials have been examined to find the best reaction system for cancrinite formation under low temperatures and pressures (473 K, autogenous pressure). Additional experiments were performed at elevated conditions at 773 K and 0.15 GPa. Polycrystalline nitrate cancrinite and various amounts of unchanged educts were obtained in all low-temperature experiments. In contrast, in the high-temperature/high-pressure experiments a crossover of sodalite and cancrinite formation was observed as a function of the Si/Al ratio within the starting system for x = 1.0, 2.0, 4.0 and 6.0 (i.e. at Si/Al ratios of 0.5, 1.0, 2.0 and 3.0). Structural investigations of nitrate cancrinite were performed by IR and MAS NMR spectroscopy of the nuclei 29Si, 27Al and 23Na. The results confirmed the alternating Si, Al ordering of the alumosilicate framework for a Si/Al ratio of 1.0 for all samples, independent of the Si/Al ratio of the educts as well as the temperature and pressure of crystallization. A distribution of the quadrupolar interaction of the sodium cations caused by the enclathrated water molecules and motional effects can be suggested from the 23Na MAS NMR spectrum. The single line with its slightly asymmetric shape makes it impossible to distinguish the sodium cations inside the structure channel from those located in the ε-cages of the cancrinite structure. In order to complete the study on nitrate cancrinite a single crystal structure refinement was carried out. As in the case of carbonate cancrinite, NO3- anions are distributed over two nonequivalent positions in the hexagonal channel of the framework. All the crystal water molecules were found to be arranged in the ε-cages of the cancrinite structure.

ASJC Scopus subject areas

Cite this

Synthesis, X-ray diffraction and MAS NMR characteristics of nitrate cancrinite Na7.6[AlSiO4]6(NO3)1.6(H2O)2. / Buhl, Josef Christian; Stief, Frank; Fechtelkord, Michael et al.
In: Journal of alloys and compounds, Vol. 305, No. 1-2, 06.06.2000, p. 93-102.

Research output: Contribution to journalArticleResearchpeer review

Buhl JC, Stief F, Fechtelkord M, Gesing TM, Taphorn U, Taake C. Synthesis, X-ray diffraction and MAS NMR characteristics of nitrate cancrinite Na7.6[AlSiO4]6(NO3)1.6(H2O)2. Journal of alloys and compounds. 2000 Jun 6;305(1-2):93-102. Epub 2000 May 10. doi: 10.1016/S0925-8388(00)00724-6
Buhl, Josef Christian ; Stief, Frank ; Fechtelkord, Michael et al. / Synthesis, X-ray diffraction and MAS NMR characteristics of nitrate cancrinite Na7.6[AlSiO4]6(NO3)1.6(H2O)2. In: Journal of alloys and compounds. 2000 ; Vol. 305, No. 1-2. pp. 93-102.
Download
@article{831b8de6311649c793c00037816ff969,
title = "Synthesis, X-ray diffraction and MAS NMR characteristics of nitrate cancrinite Na7.6[AlSiO4]6(NO3)1.6(H2O)2",
abstract = "Investigations on the hydrothermal formation and the crystal structure of nitrate cancrinite have been carried out in the system Na2O-xSiO2-Al2O3-NaNO3-H2O, 129Si, 27Al and 23Na. The results confirmed the alternating Si, Al ordering of the alumosilicate framework for a Si/Al ratio of 1.0 for all samples, independent of the Si/Al ratio of the educts as well as the temperature and pressure of crystallization. A distribution of the quadrupolar interaction of the sodium cations caused by the enclathrated water molecules and motional effects can be suggested from the 23Na MAS NMR spectrum. The single line with its slightly asymmetric shape makes it impossible to distinguish the sodium cations inside the structure channel from those located in the ε-cages of the cancrinite structure. In order to complete the study on nitrate cancrinite a single crystal structure refinement was carried out. As in the case of carbonate cancrinite, NO3- anions are distributed over two nonequivalent positions in the hexagonal channel of the framework. All the crystal water molecules were found to be arranged in the ε-cages of the cancrinite structure.",
author = "Buhl, {Josef Christian} and Frank Stief and Michael Fechtelkord and Gesing, {Thorsten M.} and Uwe Taphorn and Claudia Taake",
year = "2000",
month = jun,
day = "6",
doi = "10.1016/S0925-8388(00)00724-6",
language = "English",
volume = "305",
pages = "93--102",
journal = "Journal of alloys and compounds",
issn = "0925-8388",
publisher = "Elsevier BV",
number = "1-2",

}

Download

TY - JOUR

T1 - Synthesis, X-ray diffraction and MAS NMR characteristics of nitrate cancrinite Na7.6[AlSiO4]6(NO3)1.6(H2O)2

AU - Buhl, Josef Christian

AU - Stief, Frank

AU - Fechtelkord, Michael

AU - Gesing, Thorsten M.

AU - Taphorn, Uwe

AU - Taake, Claudia

PY - 2000/6/6

Y1 - 2000/6/6

N2 - Investigations on the hydrothermal formation and the crystal structure of nitrate cancrinite have been carried out in the system Na2O-xSiO2-Al2O3-NaNO3-H2O, 129Si, 27Al and 23Na. The results confirmed the alternating Si, Al ordering of the alumosilicate framework for a Si/Al ratio of 1.0 for all samples, independent of the Si/Al ratio of the educts as well as the temperature and pressure of crystallization. A distribution of the quadrupolar interaction of the sodium cations caused by the enclathrated water molecules and motional effects can be suggested from the 23Na MAS NMR spectrum. The single line with its slightly asymmetric shape makes it impossible to distinguish the sodium cations inside the structure channel from those located in the ε-cages of the cancrinite structure. In order to complete the study on nitrate cancrinite a single crystal structure refinement was carried out. As in the case of carbonate cancrinite, NO3- anions are distributed over two nonequivalent positions in the hexagonal channel of the framework. All the crystal water molecules were found to be arranged in the ε-cages of the cancrinite structure.

AB - Investigations on the hydrothermal formation and the crystal structure of nitrate cancrinite have been carried out in the system Na2O-xSiO2-Al2O3-NaNO3-H2O, 129Si, 27Al and 23Na. The results confirmed the alternating Si, Al ordering of the alumosilicate framework for a Si/Al ratio of 1.0 for all samples, independent of the Si/Al ratio of the educts as well as the temperature and pressure of crystallization. A distribution of the quadrupolar interaction of the sodium cations caused by the enclathrated water molecules and motional effects can be suggested from the 23Na MAS NMR spectrum. The single line with its slightly asymmetric shape makes it impossible to distinguish the sodium cations inside the structure channel from those located in the ε-cages of the cancrinite structure. In order to complete the study on nitrate cancrinite a single crystal structure refinement was carried out. As in the case of carbonate cancrinite, NO3- anions are distributed over two nonequivalent positions in the hexagonal channel of the framework. All the crystal water molecules were found to be arranged in the ε-cages of the cancrinite structure.

UR - http://www.scopus.com/inward/record.url?scp=0033733094&partnerID=8YFLogxK

U2 - 10.1016/S0925-8388(00)00724-6

DO - 10.1016/S0925-8388(00)00724-6

M3 - Article

AN - SCOPUS:0033733094

VL - 305

SP - 93

EP - 102

JO - Journal of alloys and compounds

JF - Journal of alloys and compounds

SN - 0925-8388

IS - 1-2

ER -