A method based on the sorption of99mTc in MEK on an acid alumina column has been investigated. A number of parameters as column dimension, amount of alumina, MEK volumes, etc. is found to affect the extent of adsorption and the final purity of99mTc solution. These parameters have been standardized and a method for rapid recovery of MEK-extracted99mTc has been developed. The final characteristics of the99mTc is found to conform to pharmacopoeia specification.