The available six types of Sephadex and one type of Sepharose have been applied in the separation of technetium fractions in99mTc-labelled radiopharmaceuticals produced in our laboratory using the GCS technique. By this technique the chemical state and the percentage of99mTc-fractions have been determined. The resolution efficiency of some gel types were found to be significantly influenced by the pH of the eluent. The results obtained from the experiments indicated that Sephadex G-25 Fine was the best and can be routinely used in the radiochemical analysis of the following kits:99mTc-HSA,99mTc-DTPA and99mTc-HIDA and G-100 for99mTc-PYP. With99mTc-HSA and99mTc-PYP kits, 0.9% NaCl eluents at pH 3.2 and pH 2 to 2.5, respectively, were found to be necessary for the separation of99mTc-fractions. G-50 Fine was found to be the best gel between the others in the separation of99mTc-fractions in testing of the weak radiopharmaceuticals,99mTc-GH and99mTc-MDP. The development of99mTc-MDP with the eluent at the same pH as the preparation gives negligible interaction effect.