Perchlorate enclathrated sodalite with gallosilicate host framework has been synthesized under low temperature (100 o 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 29 Si and 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 4 -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 144.036 o .The surface area of single entity with stoichiometry Na 8 [GaSiO 4 ] 6 (ClO 4 ) 2 was found to be 8.385x10 -15 cm 2 /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.