研究目的
To develop a direct, simple, and safe micro-analytical method for determining plutonium using Total Reflection X-ray Fluorescence (TXRF) spectrometry that avoids the need for glove box containment and minimizes sample handling risks.
研究成果
The developed TXRF method provides a direct, safe, and micro-analytical approach for plutonium determination with good precision and accuracy. It eliminates the need for glove box containment, reduces sample consumption and radioactive waste, and is applicable to hazardous materials. Future studies could extend this to other elements and real-world samples.
研究不足
The method is limited to plutonium determination and may have slightly higher detection limits for low atomic number elements due to the collodion layer. Sample amounts must not exceed 160 ng of Pu to avoid matrix effects, and the technique requires careful handling to prevent contamination, though risks are minimized.
1：Experimental Design and Method Selection:
The study designed a novel method using TXRF spectrometry with collodion isolation to fix plutonium samples on quartz supports, enabling safe handling in ambient air. Theoretical models for TXRF analysis were applied, focusing on minimizing matrix effects and ensuring sample stability.
2：Sample Selection and Data Sources:
Synthetic samples of plutonium were prepared from a stock solution (101.84 mg/mL Pu) with internal standards (yttrium and gallium). Multi-element standard solutions and uranium samples were used for feasibility studies. Samples were prepared with specific concentrations as detailed in tables.
3：84 mg/mL Pu) with internal standards (yttrium and gallium). Multi-element standard solutions and uranium samples were used for feasibility studies. Samples were prepared with specific concentrations as detailed in tables.
List of Experimental Equipment and Materials:
3. List of Experimental Equipment and Materials: Quartz TXRF sample supports, collodion solution (10% in amyl acetate), plutonium stock solution, internal standards (yttrium and gallium), fume hood, protective clothing, hand gloves, thermoluminescence dosimeters, TXRF spectrometer (low Z–high Z model from Atominstitut, Vienna), alpha spectrometer (PIPS detector from Canberra), and various chemicals from suppliers like SD Fine Chem Limited.
4：Experimental Procedures and Operational Workflow:
Sample solutions (2 μL aliquots) were deposited on quartz supports and dried. A 10 μL drop of 10% collodion solution was applied to cover the sample spot, forming a protective layer. Operations were conducted inside a fume hood with radiological precautions. Specimens were wiped clean, checked for alpha activity, and measured using TXRF and alpha spectrometry with specified counting times.
5：Data Analysis Methods:
TXRF spectra were processed using EDXRF32 software. Peak areas and intensities were analyzed for elemental quantification. Statistical methods included calculation of precision (standard deviation) and deviation from expected values. Alpha spectrometry data were analyzed using PCA3 software for peak area integration.
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