Synthesis, Characterization and Crystal Structure of Gallosilicate Perchlorate Sodalite

Perchlorate enclathrated sodalite with gallosilicate host framework has been synthesized under low temperature (100 degree C) 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 super( 29)Si and super( 23)Na nuclei and by Reitveld refinement of X-ray powder diffraction data. IR and Raman spectroscopy confirms formation of framework and presence of ClO sub( 4) super( -) 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 Aa, V = 768.5 Aa, Z =1, Rwp = 0.0611, Rp = 0.1079 and Si-O-Ga is 144.036 degree . The surface area of single entity with stoichiometry Na sub( 8)[GaSiO sub( 4)] sub( )sub 6 (ClO sub( 4)) sub( 2) was found to be 8.385x10 super( -15) cm super( 2)/g. super( 29)Si 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.