JAST
2012 March;3(1):95-103.
Published online 2012 January 17.
doi:http://dx.doi.org/10.5355/JAST.2012.95
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| Copyright ⓒ 2010 Journal of Analytical Science & Technology |
| Synthesis and characterization of perchlorate enclathrated aluminogermanate sodalite and its potassium and silver derivatives |
| Ashok Vishram Borhade*, Arun Gabaji Dholi, Dipak Ramrao Tope, Sanjay Gauram Wakchaure |
| Research Centre and Department of Chemistry, HPT Arts and RYK Science College, Nasik 422005, India |
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Corresponding Author:
Ashok Borhade ,Tel: O9421831839, Email: ashokborhade2007@yahoo.co.in |
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ABSTRACT |
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| Perchlorate enclathrated sodalite with aluminogermanate host framework has been obtained from low temperature hydrothermal synthesis at 373K. In addition mixed sodium, potassium and silver perchlorate sodalite is obtained by aqueous cation exchange method. The crystal structure of Na8[AlGeO4]6(ClO4)2, Na3.2K4.8[AlGeO4]6(ClO4)2 and Na3.9Ag4.1[AlGeO4]6(ClO4)2 sodalites were refined from X-ray powder data in the space group P 3n: a = 9.249 Å, V = 791.35 Å, Rwp = 0.2230, Rp = 0.1609 and Al-O-Ge angle is 140.930o and a = 9.257 Å, V = 793.28 Å, Rwp = 0.1596, Rp = 0.1180 and Al-O-Ge angle is 141.080o, a = 9.195 Å, V = 775.95 Å, Rwp = 0.2211, Rp = 0.1662 and Al-O-Ge angle is 139.034o ,respectively. The 27Al MAS NMR study confirms alternating Ge and Al ordering of sodalite framework, while 23Na give insights into the structure and dynamics of the cage fillings. The recorded Infrared and Raman spectra show absorption band typical for the sodalite structure. Thermogravimetric analysis has provided information on the extent of perchlorate entrapment, stability within the sodalite cage and decomposition properties. SEM study shows the retention of cubical morphology of the sodalite derivatives.
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| Keywords: Hydrothermal method, Aluminogermanate sodalite, Cation exchange, IR shift, Rietveld refinement, MAS NMR |
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