Methods of separation and quantification by ICP-MS for Pd-107 in radioactive waste

Abstract The goal of this study was to improve the current method used to characterize radioactive waste for dismantling and decommissioning applications. In particular, a focus was made on the method for the separation of palladium from other radionuclides. A purification procedure based on extraction chromatographic Ni-resin® for Pd-107 analysis was investigated on non-radioactive commercial standard solutions. It was developed from a design of experiment method using a screening design to recover the palladium entirely. An additional step with LN-resin® was introduced to achieve a better selectivity. The complete method consisting of sample digestion, filtration, and the combination of these two resins showed a good palladium recovery at 85%. The optimized procedure was applied on real radioactive waste (effluents and sludges). The specificity and efficiency of this new separation were compared with those obtained with the current reference procedure used in our laboratory. As a result, the new validated protocol successfully replaced the liquid–liquid extraction in chloroform and separation by anion exchange chromatography implemented in the existing method. This study also includes a comparison between two quantification methods by single quadrupole ICP-MS: one based on a standard of natural Pd and the other one based on a Pd-107 standard.