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Methods for preparation of working plutonium nitrate calibration and test material (CTM) solutions similiar to typical nuclear fuel cycle solutions are described. These working CTM solutions are to be used in calibrating and providing quality control surveillance of analytical methods for measurement of plutonium assay and isotopic abundances. Source materials are prepared from NBS plutonium certified reference materials, highly pure plutonium metal, or plutonium nitrate obtained from a plant inventory. Some solutions are prepared for assay measurement only, some for isotopic abundance measurement only, and others for both purposes. Procedures are described for their packaging and storing as evaporated slurry, solution for shortterm storage, and solution for long-term storage. Analytical overcheck and characterization procedures are suggested, and statistical tests to assess the reliability of the working CTM solutions are given. This report outlines methods for preparing working plutonium nitrate calibration and test solutions similar to nitrate solutions in the nuclear fuel cycle. These working solutions are to be used in calibration and quality control surveillance of analytical me~ods recommended for assay and isotopic

Preparation of working calibration and test materials for intra- and interlaboratory surveillance of nuclear materials measurement methods: plutonium nitrate solution