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Related Experiment Video

Updated: Apr 14, 2026

Atom Probe Tomography Analysis of Exsolved Mineral Phases

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Sample preparation for actinide isotopic analysis using FIB-SEM.

A D Wood¹, S A Dunn², P Kaye²

¹Department of Mechanical and Aerospace Engineering, School of Engineering, University of Manchester, Oxford Road, Manchester, England.

Journal of Radioanalytical and Nuclear Chemistry

|April 13, 2026

Summary

This summary is machine-generated.

Researchers developed methods to analyze tiny uranium dioxide (UO2) samples for isotopic composition. This advancement enables precise spatial isotopic analysis of nanogram-scale radioactive materials.

Keywords:

Actinide analysis Focussed ion beam Mass spectroscopy Nuclear forensics Radiochemistry

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Area of Science:

Nuclear Chemistry
Materials Science
Analytical Chemistry

Background:

Accurate isotopic analysis of uranium dioxide (UO2) is crucial for nuclear fuel cycle applications.
Existing techniques often require larger sample sizes, limiting spatial resolution.
The need for sensitive methods to analyze nanogram-scale samples of radioactive materials persists.

Purpose of the Study:

To establish capabilities for extracting and analyzing nanogram-scale UO2 samples for spatial isotopic analysis.
To adapt existing techniques for handling alpha-emitting radioactive materials.
To assess the precision and accuracy of isotopic measurements on micro-samples.

Main Methods:

Utilized a Helios 5CX Focused Ion Beam Scanning Electron Microscope (FIB-SEM) adapted for radioactive materials to extract 2-80 ng UO2 samples from a depleted pellet.
Employed Thermal Ionization Mass Spectrometry (TIMS) for isotopic composition analysis.
Applied Triple Quadrupole Inductively Coupled Mass Spectrometry (ICP-QQQ-MS) for isotopic ratio measurements.

Main Results:

TIMS successfully measured weight percentages of 234U, 235U, 236U, and 238U with relative standard uncertainties (RSU) ranging from 0.26% to 11%.
ICP-QQQ-MS determined the 235U/238U ratio with an RSU of 37.4%.
Demonstrated feasibility of isotopic analysis on sub-microgram UO2 samples.

Conclusions:

Developed and validated a methodology for spatial isotopic analysis of nanogram-scale UO2 samples.
The established techniques provide valuable data for understanding material composition at a micro-scale.
This work advances the field of nuclear material characterization and safeguards.