The reactions between Co/sup 2 +/ and different thiomolybdate anions (MoS/sup 2 -//sub 4/, Mo/sub 4/S/sup 6 -//sub 15/, Mo/sub 2/S/sup 2 -//sub 7/ and Mo/sub 4/S/sup 2 -//sub 13/) have been investigated by means of glass electrode and conductometric titrations between the reactants at several concentrations. The results provide definite evidence for the formation of CoS.MoS/sub 3/ and 3CoS.4MoS/sub 3/ around pH 7.1 and 5.9, respectively. The titrations of cobalt chloride with Na/sub 2/S.2MoS/sub 3/ and Na/sub 2/S.4MoS/sub 3/ failed to provide any dependable results for the formation of the corresponding cobalt thiomolybdates. The accuracy and reproducibility of these titrations are of high order. Analytical investigations of these compounds have also been carried out and substantiate the results of the pH and conductometric measurements.