A simple separation technique of (99m)Tc from Na(2)[(99)Mo]MoO(4) in sodium hydroxide solution obtained from the (98)Mo(n,gamma)(99)Mo reaction is described. Low to medium specific activity (99)Mo-molybdate solution of 7.4-18.5GBq (200-500mCi) in sodium hydroxide was passed through a tiny Dowex-1 column (25mg) to separate the (99m)Tc from the (99)Mo; subsequently the (99m)Tc was eluted from the Dowex 1 column with tetrabutylammonium bromide (TBAB) solution (1mg/5ml methylene chloride). The TBAB solution was passed through a small alumina column (1.5g) where the (99m)Tc is retained and separated from TBAB and CH(2)Cl(2). Technetium-99m from the alumina column was finally eluted with 5ml saline leaving any traces of (99)Mo on the alumina column. The separation yield was about 90% (n=10). The method has applicability for decontamination of (99g)Tc from spent (99)Mo waste solution and recovery of (99g)Tc for research use. The procedure should also be equally applicable for recovery of (188)ReO(4) from (188)WO(4) in a radioisotope laboratory.