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Microextraction–TQ–ICP–MS for the Direct Analysis of U and Pu from Cotton Swipes

  • Veronica C. Bradley
    Veronica C. Bradley
    Chemical Sciences Division, Oak Ridge National Laboratory, Oak Ridge, Tennessee 37831, United States
  • Brian W. Ticknor
    Brian W. Ticknor
    Chemical Sciences Division, Oak Ridge National Laboratory, Oak Ridge, Tennessee 37831, United States
  • Daniel R. Dunlap
    Daniel R. Dunlap
    Chemical Sciences Division, Oak Ridge National Laboratory, Oak Ridge, Tennessee 37831, United States
  • N. Alex Zirakparvar
    N. Alex Zirakparvar
    Chemical Sciences Division, Oak Ridge National Laboratory, Oak Ridge, Tennessee 37831, United States
  • Shalina C. Metzger
    Shalina C. Metzger
    Chemical Sciences Division, Oak Ridge National Laboratory, Oak Ridge, Tennessee 37831, United States
  • Cole R. Hexel
    Cole R. Hexel
    Chemical Sciences Division, Oak Ridge National Laboratory, Oak Ridge, Tennessee 37831, United States
  • , and 
  • Benjamin T. Manard*
    Benjamin T. Manard
    Chemical Sciences Division, Oak Ridge National Laboratory, Oak Ridge, Tennessee 37831, United States
    *Email: [email protected]
Cite this: Anal. Chem. 2023, 95, 43, 15867–15874
Publication Date (Web):October 6, 2023
https://doi.org/10.1021/acs.analchem.3c01022
Copyright © 2023 American Chemical Society

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    Abstract

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    The microextraction sampling technique was integrated with triple quadrupole─inductively coupled plasma–mass spectrometry (TQ–ICP–MS) to directly sample and measure the isotopic compositions of uranium (U) and plutonium (Pu) from cotton swipes. Once extracted, the U/Pu were directed into the TQ–ICP–MS instrument for isotopic determination. Carbon dioxide (CO2) and helium (He) gases were delivered to a collision reaction cell within the ICP–MS system for ion separation. The CO2 reacts with the U+ forming UO+ which is ultimately separated from the Pu+ ions of interest in the third quadrupole. This study demonstrates direct liquid extraction of U/Pu from a solid surface and subsequent measurement by TQ–ICP–MS in <60 s. Flow rates were optimized (0.3 mL min–1 CO2 and 5 mL min–1 He) in the reaction cell of the ICP–MS system to maximize the Pu signal while minimizing U interferences (i.e., 238U+ tail and 238UH+) at m/z 239. Low levels of Pu (∼2 pg) were deposited on a cotton swipe along with U at concentrations ranging from 20 to 200 ng. The 240Pu/239Pu ratio was measured with <7% relative difference from the certified value at all U concentrations. Major and minor U isotope ratios were also measured with <4% relative difference. This highlights that the microextraction–TQ–ICP–MS method can extract a mixed U/Pu sample directly from a cotton swipe and measure both isotopic systems without chemical separation.

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