Synthesis of Decaammine-μ-peroxo-dicobalt disulfate

To a solution prepared by dissolving 6.6 g of ammonium sulfate in 50 mL of water, 100 mL of concentrated ammonia is added with stirring, whereto after 5 minutes 100 mL of water is added. A separate solution is prepared from 14.06 g of cobalt sulfate heptahydrate and 50 mL of water, is added slowly over the course of 5 minutes. Then a solution prepared from 5.5 mL of concentrated hydrogen peroxide in 50 mL of water is added to the mixture with stirring. Lastly, a solution prepared from 11.45 g of ammonium sulfite in 50 ml of water is added to the mixture. The mixture is left to stir for 15 minutes, filtered, washed with some aq. ammonia and ethanol, and left to dry on the pump. The residue is recrystallized from hot 150 mL of a 2N solution of sulfuric acid.  The product is obtained as a trihydrate.

(NH3)5CoO2Co(NH3)5(SO4)·4H2O

Source

Addition of the reagents

The crude product

The recrystallized product

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