Direct Multielemental Trace Determinations in Plutonium Samples by Total Reflection X-ray Fluorescence Spectrometry...

Area of Science:

• Analytical Chemistry
• Nuclear Chemistry
• Spectroscopy

Background:

• Plutonium sample analysis typically requires gloveboxes due to radioactivity.
• Conventional methods for trace element determination in plutonium can be cumbersome and involve significant radioactive waste.
• There is a need for simpler, safer, and more sensitive analytical techniques for plutonium samples.

Purpose of the Study:

• To develop a simple, safe, and sensitive method for direct multielemental trace determinations in plutonium samples.
• To avoid the need for glovebox operations in plutonium sample analysis.
• To minimize radiation dose and radioactive waste management issues.

Main Methods:

• Utilized total reflection X-ray fluorescence (TXRF) spectrometry.
• Separated the plutonium matrix from sample solutions.
• Deposited a small volume (2 μL) of sample solution onto TXRF supports for direct analysis.
• Analyzed samples using TXRF spectra, internal standards (Se or Ga), and predetermined sensitivity values.

Main Results:

• Achieved elemental detection limits for K-Sr ranging from 1.06 to 0.09 ng.
• Successfully analyzed elements K, Ca, Cr, Mn, Fe, Ni, Cu, Zn, Sr, Ba, Tl, and Pb at μg/mL levels.
• Obtained an average relative standard deviation (RSD) of 4.5% for prepared samples and 10.6% for real plutonium samples.
• Demonstrated results comparable to conventional techniques with added safety and operational advantages.

Conclusions:

• The developed TXRF method offers a simple, safe, and sensitive approach for direct multielemental trace analysis of plutonium.
• This method eliminates the need for glovebox handling, reducing operational complexity and radiation exposure.
• The technique is effective for analyzing trace elements in both prepared and real plutonium samples, providing reliable results with reduced environmental and safety concerns.