DOE OSTI2021
The goal of the salt sampling program at Argonne is to develop and deploy automated molten salt sampling approaches for interfacing relevant unit operations with salt analysis to improve the timeliness of sampling-based accountancy measurements. Two technologies under development in support of this goal are a vacuum sampling loop module and a high-throughput pneumatic sample generator module. Compared to traditional point sampling approaches (i.e., dip probes), the vacuum sampling loop facilitates the collection of a larger cross-section of the bulk salt in order to collect more representative samples. The vacuum sampling approach also eliminates the risk of dross contamination of samples and avoids the use of moving parts in the salt. The pneumatic sample generator module is used to facilitate high-throughput sample analysis to improve the measurement precision of any given analytical technique by averaging out random sampling and measurement errors. In FY21, two methods for integrating these two modules were tested including direct fluidic coupling and coupling using a solid salt transfer mechanism. Solid salt transfer was ultimately selected over fluidic coupling, primarily to enable the transport of samples over longer distances to support automated at-line integration with high-precision techniques (such as microcalorimetry) that cannot withstand the conditions near an electrorefining process. To facilitate rapid solid salt coupling, new mechanisms were developed for rapidly charging and discharging salt sample tubes at the vacuum sampling loop and pneumatic sample generator modules, respectively. While the charging mechanism will be deployed in FY22, the discharge mechanism was tested in FY21 and is described here. The solid salt tube transfer method was deployed at one of Argonne’s engineering-scale electrorefiners to implement at-line high-throughput pneumatic micro-sample generation capabilities. The approach was used to generate precise uranium- and lanthanide-bearing electrorefiner micro-samples with the specific dimensions requested by researchers at Los Alamos National Laboratory for use in testing their novel microcalorimeter x-ray techniques. The solid salt transfer mechanism proved not only to be an effective means of integrating the precision sample generator with vacuum sampling, but also improved the performance of the sampler generator. To discharge salt from the sample tubes at the sampler generator, tube segments were inserted directly into the sample generator’s Helmholtz chamber and pressure pulse actuations were used to generate precision molten salt samples directly from the tube segments. The direct insertion of sample tubes into the sample generator enabled rapid loading of the salt and prevented salt from contacting most of the interior surfaces of the sample generator, which eliminated cross-contamination between runs. The vacuum sampling-loop tube charging mechanism will support high-throughput tube sampling operations by employing a dynamic vacuum filling process to fill short charge tubes that are configured to be rapidly connected and disconnected from the loop. The dynamic vacuum sampling operation will be automated, and sample tube handling can be executed with simple overhead actuation. Because the modular sampling approach described here eliminates the need for new high-radiation sample handling capabilities, salt-wetted seals, salt-wetted moving parts, and heated transfer lines outside the electrorefiner, it will address most of the remaining technical challenges for the at-line deployment of high-precision analytical techniques which will enable significant reductions in the time delay for sampling-based high-precision accountancy measurements.