Separation of high purity In-111 from irradiated Cadmium targets for medical purposes is the major aim of this work. To this end, various experiments using the Solid Phase Extraction (SPE) methods have been documented in this research. This thesis illustrates a fast and convenient way for further purification of 111In solutions shortly before their use. Means of selective recovery of highly enriched 112Cd from dissolved targets is also provided, since highly enriched 112Cd is expensive. Weight distribution ratios (Dw values), as a measure of the distribution behavior of Indium and Cadmium on different SPE materials in different acids or acid/salt mixtures of varying concentrations have been determined to arrive at optimal conditions for separation and purification of carrier-free In-111 from irradiated Cadmium targets. Elution studies have been undertaken to examine the behaviour of Cadmium and Indium isotopes on four commercially available SPE materials--TEVA Resin®, TRU Resin®, Ln Resin® and Ac Resin® all of which are manufactured by Eichrom Technologies, Inc. These resins have been thoroughly examined towards their usefulness for achieving the above mentioned goals.