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Carrier free 111Ag has been separated from neutron irradiated palladium targets by the combined co‐crystallisation and electrodeposition techniques. Co‐crystallisation coefficient measurements of silver activity on NaCl were performed, and the best condition for the separation of Ag‐111 in more than 90% yield was carried out. The method requires no consumption of special chemicals and renders the quantitative separation and subsequent use of irradiated palladium possible. The purification of target before irradiation by solvent extraction eliminates radiochemical impurities expected from trace metals in the original target, particularly gold and silver. The product separated proved to be of high chemical and radiochemical purity.

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