To shorten lengthy and costly manual chemical purification procedures, sample preparation methods for mass spectrometry are being automated using commercial-off-the-shelf (COTS) equipment. This addresses a serious need in the nuclear safeguards community to debottleneck the separation of U and Pu in environmental samples—currently performed by overburdened chemists—with a method that allows unattended, overnight operation. In collaboration with Elemental Scientific Inc., the prepFAST-MC2 was designed based on current COTS equipment that was modified for U/Pu separations utilizing Eichrom™ resins. Initial verification of individual and combined columns yielded small elution volumes, consistent elution profiles, ample separation, and good recovery without cross-contamination of the eluent. Optimization of the packing and unpacking methods led to a reduction in the variability of the packed resin from &gt;15% to &lt;5% daily. The reproducibility of the automated system was tested with multiple samples containing 30ng U and 15pg Pu, which were separated in a series with alternating reagent blanks. Washout of both the resin and sample from the columns was evidenced by low blank values. Analysis of the isotope ratios for U and Pu provided values well within data quality limits for the IAEA. Additionally, system process blanks spiked with 233-U and 244-Pu tracers were separated after the system was moved outside of a clean room and yielded levels equivalent to clean room blanks, confirming that the system can produce high quality results without the need for expensive clean room infrastructure. Comparison of the amount of personnel time necessary for successful manual vs. automated chemical separations showed a significant decrease in hands-on time from 9.8 h to 35 min for 7 samples, respectively. This documented time savings and reduced labor translates to significant cost savings per sample. Overall, the system will enable faster sample reporting times with reduced costs by limiting personnel hours dedicated to the chemical separation.

Automated clean chemistry for bulk analysis of environmental swipe samples

253rd National Meeting (2017)

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