SummaryUranium metal, which is present in sludge held in the Hanford Site K West Basin, can create hazardous hydrogen atmospheres during sludge handling, immobilization, or subsequent transport and storage operations by its oxidation/corrosion in water. A thorough knowledge of the uranium metal concentration in sludge therefore is essential to successful sludge management and waste process design.The goal of this work was to establish a rapid routine analytical method to determine uranium metal concentrations as low as 0.03 wt% in sludge even in the presence of up to 1000-fold higher total uranium concentrations (i.e., up to 30 wt% and more uranium) for samples to be taken during the upcoming sludge characterization campaign and in future analyses for sludge handling and processing. This report describes the experiments and results obtained in developing the selective dissolution technique to determine uranium metal concentration in K Basin sludge. The work described in this report:• provides a technical underpinning of the validity of the selective dissolution method, including the influence of various sludge components, in five test series using simulated and genuine sludges of widely varying composition• establishes analytical parameters (concentrations, quantities, temperatures, and times) necessary to develop the selective dissolution sludge-digestion analytical procedure.The uranium metal detection limit is estimated to be about 0.004 wt% based on the testing performed with actual sludge, thus meeting the goal detection limit of 0.03 wt%. The detection limit largely is established by the trace residual uranium carryover that exists in the leached and rinsed sludge. In the final series of method validation tests using actual K Basin sludge, spiked with uranium metal at concentrations ranging from 0.025 to 1.29 wt%, uranium metal recoveries averaged 99.4% with a standard deviation of 3.3%.