Year
2023
File Attachment
finalpaper_156_0511020304.pdf600.17 KB
Abstract
The determination of uranium and plutonium isotopic abundance on environmental samples
collected by International Atomic Energy Agency (IAEA) inspectors is vital for the detection of
undeclared nuclear activities and material under the international nuclear safeguards regime. Current
analytical protocols require time-consuming sample preparation steps prior to subsequent
measurement by inorganic mass spectrometry (MS). Recent efforts from this laboratory have focused
on developing sample preparation methods for faster analysis, potentially allowing higher sample
throughput[1]. Alternative methods including microextraction sampling in conjunction with
inductively coupled plasma-mass spectrometry (ICP-MS) have been recently explored. This
methodology, microextraction-ICP-MS, was developed such that uranium and plutonium could be
extracted from the swipe surface and directed into the ICP-MS for an in-situ measurement,
eliminating the need for swipe ashing and digestion. A commercial off-the-shelf microextraction
system was customized with an automated movable XY stage that can be programmed to save
sampling locations, allowing for automated rapid sampling of swipe surfaces. Additional efforts have
focused on the utilization of collision cell technology to the microextraction ICP-MS method. This
would eliminate the need for lengthy column chemistry procedures to purify separated uranium and
plutonium fractions before analysis. Here, the extracted U/Pu analyte is measured by reacting the
uranium ions with CO2 in the collision cell of an ICP-MS, shifting the uranium to UO+
, which would
not interfere with the plutonium isotopic determination. The developed method utilizing collision
cell – ICP-MS technology has demonstrated the ability to measure plutonium isotope ratios in the
presence of high uranium concentration on the transient signal from the microextraction system.