The adsorption behaviour of more than 50 ions has been studied under dynamic conditions on nickel ferrocyanide in various aqueous solutions of hydrochloric, nitric, perchloric, acetic, hydrofluoric acids of 1M molarity and in a mixture of 40% 2.5M hydrochloric acid and 60% acetone. Among the retained elements we found cations forming insoluble ferrocyanide salts and alkali metals. On the basis of the behaviour of each element, we have found the possibilities of some radiochemical separations, especially cesium-alkaline earth metals, arsenic-antimony, manganese-nickel in hydrochloric solution, molybdenum-technetium in acetic solution. In order to choose the best conditions, distribution coefficients have been measured as a function of acid molarity in the 0.01M–2M range. These separations were used for the activation analysis of various metals, for example the determination of nickel in chromium and iron. An exchange system has been developed to retain the silver matrix quantitatively in the determination of manganese in this metal.