A new method for the extraction and spectrophotometric determination of La(III), Pr(lII), Nd(III), Sm(III), Gd(III) and Tb(III) from dilute aqueous nitrate media by 2-mercapto-4, 4, 6-trimethyl-(1H, 4H)-pyrimidine-1-acetic acid (MTPAcH) has been developed. Various polar organic solvents have been examined. Maximum enhancement is observed in the presence of 40% acetonitrile. Very poor extractability necessitated the use of calcium nitrate as the salting out agent.