Los Alamos National Laboratory (LANL) successfully polished 120kg of plutonium from surplus nuclear weapons for the European Mixed Oxide (MOX) Lead Test Assembly (LTA), managed by Duke, COGEMA, and Stone & Webster (DCS). The purified oxide was fabricated into fuel pellets, which comprised the LTAs. The LTAs have been inserted into the Catawba (SC, USA) nuclear reactor, where they are presently being used to generate electricity. The material used in the MOX LTA represents the first plutonium oxide from LANL to be polished under the quality requirements set forth by the Nuclear Regulatory Commission (NRC). In addition, the MOX project has been hailed as the “largest single nonproliferation project in history” by US Ambassador Linton Brooks (23/9/04). The process flow for PuO2 purification was based on aqueous recovery that included various unit operations (dissolution, ion exchange, oxalate precipitation, and calcination). Data from a variety of chemical and physical analyses demonstrate product quality and process consistency. Further process optimization experiments will be performed prior to polishing an additional 330kg of PuO2 for the Mixed Oxide Fuel Fabrication Facility (MFFF) at Savannah River Site. During LTA production in 2004, approximately 500L of 7M nitric acid was used for washing impurities from the plutonium in order to meet product purity specifications. The majority of this acid was sent to the LANL Radioactive Liquid Waste Treatment Facility (TA-50) as effluent. Optimization experiments during 2006 and 2007 will investigate the use of recycled HNO3 for PuO2 washing and ion exchange. If successful, aqueous polishing processes will re-use almost all of the nitric acid that would otherwise have been sent to TA-50. In addition, an overall reduction in the volume of nitric acid used during ion exchange will be tested. The use of new Inconel calcination boats will also be verified. Additional process optimization activities will be conducted to validate the use of 100% quaternized Reillex ion exchange resin. Qualification exercises will include a series of process runs, followed by chemical analyses to assess product oxide impurity levels. Once the optimized processes have been qualified, the production phase of the project will begin.