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The thermal decomposition in argon of the monohydrated ammonium tris(oxalate)niobate, (NH 4 ) 3 NbO(C 2 O 4 ) 3 .H 2 O, has been studied by TG/DTG, DTA, DSC, IR absorption and XRD. The material decomposes stepwise by the release of CO, CO 2 , NH 3 and water. The atomic structure of the complex initially becomes amorphous and then crystallizes twice in the form of orthorhombic and monoclinic niobium pentoxide.doi:10.1590/s0104-66322006000400011 fatcat:u3eum4p5brauximbb65rjsxnxi