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Detailed vibrational (IR, Raman, far-IR) and thermal (TGA, TG–MS, DSC) analysis has been performed on di[κ 1 O,κ 2 O-carbonatotetraamminecobalt(III)] sulfate trihydrate, ([Co(NH 3 ) 4 CO 3 ] 2 SO 4 ·3H 2 O ( 1 ). Its isothermic heating at 100 °C leads to formation of [Co(NH 3 ) 4 CO 3 ] 2 SO 4  (compound  2 ). UV and IR studies showed that the distorted octahedral arrangement around cis-O 2 CoN 4  core in compound  1  does not change during dehydration, which explains the reversible water loss and ability of compound  2  to rehydrate into compound  1 . Compound  2  decomposes at ~ 240 °C in inert atmosphere giving final decomposition products, which are two modifications of nanosized metallic cobalt (hcp-15 nm, fcc-250 nm) and CoO (55 nm). The redox reaction results in N 2  as an ammonia oxidation product. The decomposition intermediate is a cobalt(II) compound, Co 2 O 1,14+δ (SO 4 ) 0.86  ( δ  = the oxygen surplus due to the presence of 2.8% of Co(III) ion). The same reaction in air atmosphere resulted in Co 2 O 1.25+δ (SO 4 ) 0.75  ( δ  = the oxygen surplus due to the presence of 5.3% of Co(III) ion (compound  3a ). Compound  3a  is oxidized in air at 793 °C into Co 3 O 4 . The compound  3a  exhibits catalytic activity in photodegradation in Congo red. The photodegradation process follows pseudo-first-order kinetic ( k  app  = 1.0 and 7.0. at pH = 3.4 and 5.25, respectively).

journal of thermal analysis and calorimetry

Thermal decomposition and spectral characterization of di[carbonatotetraamminecobalt(III)] sulfate trihydrate and the nature of its thermal decomposition products