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Synthesis of Cyclic Phosphates in Hot,Concentrated Phosphoric Acid
Authors:Swafford  Sean H  Boutfessi  Aicha  Boukhari  Ali  Holt  Elizabeth M
Institution:(1) Department of Chemistry, Oklahoma State University, Stillwater, Oklahoma, 74078;(2) Departement de Chimie, Faculté des Sciences, Laboratoire de Chimie du Solide Appliquée, B. P. 1014, Rabat, Maroc
Abstract:The synthesis of transition metal phosphates in hot, concentrated phosphoric acid medium leads to highly crystalline materials and to increased condensation of the phosphate at higher temperatures. Aluminum extraction from the porcelain crucible is also observed in some circumstances. Two new compounds were produced: (Al3.28Cr0.72)(P4O12)3 a = 13.512(8) Å, cubic, I-43d, V = 2470(3) Å3, Z = 6, density = 2.887 mg/m3, R = 0.055, GOF = 1.29 for 254 data points, was prepared at 748 K whereas (Al1.97Cr1.03)P9O27 a = b = 11.170(6), c = 9.412(9) Å, trigonal P – 3c1, V = 1017(1) Å3, Z = 2, density = 2.669 mg/m3, R = 0.0581, GOF = 0.87 for 676 data points, was produced at 798 K from the heating of Cr2O3 in H3PO4 in a porcelain crucible. Crystal structures of both materials show mixed metal sites containing Al and Cr.
Keywords:Condensed phosphates  Cr+3  crystal structure  concentrated phosphoric acid as solvent
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