The (Co1-xMnx)(3)O-4 solid solution have been synthesized in water at 60 degrees C by soda addition to a cationic solution. XRD patterns show that spinel oxide has been obtained except for pure cobalt composition which exhibits also the presence of hydroxide and oxy-hydroxide. Therefore, to reach this composition, a different synthesis route has been developed: the cationic solution is added to the soda and for the first time Co3O4 nanoparticles have been synthesized by a direct precipitation in aqueous solution at low temperature. For each composition, the particles are well crystallized and exhibit a size close to 50 nm. Each particle is composed by several crystallographic domains of about 10 nm. The cubic to tetragonal transition reported in the literature for x = 0.46 is observed in between x = 0.33 and x = 0.50. Raman spectra show that substitution of Co by Mn, in the cubic phase, introduces a random high disorder. In the tetragonal phase, occupation of the octahedral site remains a random occupation, while the tetrahedral site seems to be preferentially occupied by Co ions. All these results show that the precipitation is a simple, fast and safe process to synthesize pure phase of (Co1-xMnx)(3)O-4 spinel solid solution in aqueous media at low temperature. (C) 2017 The Society of Powder Technology Japan. Published by Elsevier B.V. and The Society of Powder Technology Japan. All rights reserved.