Americium from analytical solid waste containingUandmetallic impuritieswas separated using hollowfiber supported liquidmembrane (HFSLM) technique impregnated with DHOA–TODGA from nitric acid medium. An aliquot of 5 g of the solid waste containing Am (19.95 mg) as minor actinide and of U (2,588 mg), Fe (1,360 mg), Ca (1,810 mg) and Na (3,130 mg) as major impurities was processed. The feed solution obtained after the dissolution of the residue in ~4 MHNO₃ was passed through HFSLMmodule. In the first stage using 1 M DHOA–dodecane U was recovered while Am and other impurities were left in the raffinate. In the second stage, 0.5 MDHOA + 0.1 MTODGA/dodecane was used for the separation of Am from other impurities. Though, majority of the elements were separated in this cycle, Ca was co extracted along with the americium. CMPO extraction chromatographic technique was used for further separation of americiumfromCa. Significant decontamination factors were achieved in this three step separation process with respect to U, Fe, Na and Ca with ~77 %recovery of americium.