This work describes a streamlined approach to the recovery and purification of 234U from aged 238Pu. Key modifications to conventional techniques are described that result in an efficient uranium and plutonium separation process that successfully produced tens of grams of ultrahigh purity 234U at Oak Ridge National Laboratory. A new processing scheme was developed using an anion exchange column run in a cycling mode with HNO3 media as the primary uranium purification process. This was followed with a uranyl peroxide precipitation step to purify and solidify the uranium before conversion to U3O8. Both the traditional uranyl peroxide precipitation method and a new cascade uranyl peroxide precipitation process were used for final purification of the 234U.