Synthesis, Characterization and Crystal Structure of Gallosilicate Perchlorate Sodalite

Ashok Vishram Borhade, Arun Gabaji Dholi, Sanjay Gauram Wakchaure

Abstract


Perchlorate enclathrated sodalite with gallosilicate host framework has been synthesized under low temperature (100 oC)
hydrothermal technique and characterized by X-ray powder diffraction, IR, Raman spectroscopy, UV DRS, SEM, MAS
NMR spectroscopy and thermogravimetry. The structural features were investigated by IR, MAS NMR spectroscopy of
29Si and 23Na nuclei and by Reitveld refinement of X-ray powder diffraction data. IR and Raman spectroscopy confirms
formation of framework and presence of ClO4
- group. The tetrahedral framework T-atoms are completely ordered and
the chloride atoms are located at the centre of the sodalite cages. The crystal structure of this new sodalite was refined
in the space group P 4 3n with a = 9.15788 Å, V = 768.5 Å, Z =1, Rwp = 0.0611, Rp = 0.1079 and Si-O-Ga is 144.036o
.
The surface area of single entity with stoichiometry Na8[GaSiO4]6(ClO4)2 was found to be 8.385x10-15 cm2/g. 29Si MAS
NMR study confirms complete ordering of Si and Ga in the gallosilicate framework. Thermo gravimetric analysis has
provided information on the extent of perchlorate entrapment, stability within the cage and decomposition properties.


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International Journal of Chemistry   ISSN 1916-9698 (Print)   1916-9701 (Online)

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