A process was developed to separate milligram quantities of »"Cf from multigram quantities of 244 Cm and 218 Am with the technique of pressurized cation exchange elution chromatography. Ammonium Λ-hydroxyisobutyrate was used as the elutriant in a pn-gradient elution. An in-line radiation monitoring system gave exact elution profiles for 252 Cf, 844 Cm, 249 Am, 154 Eu, and 144 Ce.A process was developed to separate milligram quantities of 252 Cf from multigram quantities of ^Cm and 243 Am and from milligram quantities of 144 Ce and 154 Eu with the technique of pressurized cation exchange elution chromatography. Ammonium-«-hydroxyisobutyrate was used as the elutriant in a ^-gradient elution.