Destructive Analyses Techniques for Safeguards
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Transcript of Destructive Analyses Techniques for Safeguards
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Destructive Analyses Techniques for Safeguards
Mary L. Adamic
June 30, 2009
INL/CON-09-16263
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Outline
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Destructive Analysis
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Example of DA techniques
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Destructive Analysis in Safeguards
• Traditional Safeguards– SNM accountability– Assay, isotopic, and impurity measurements critical
for accurate accounting of SNM
• Environmental Safeguards– Swipe sampling in safeguarded facilities– Isotopic and assay measurements– Verification of declared operations– Detection of undeclared operations
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Advantages of DA techniques
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Comparison of precision of NDA and DA Methods
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Disadvantages of Destructive Analysis
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Timeline for NDA and DA Methods
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Traditional Safeguards DA Measurements
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Davies and Gray Uranium Assay(Redox or Electrometric Titrimetry)
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Davies and Gray Uranium Assay (cont.)
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Coulometric Plutonium Assay Titration
• Used for a wide range of materials including metals, oxides, salts and solutions.
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Coulometric Plutonium Assay Titration
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Ceric Titration for Plutonium Assay
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Ceric Titration for Plutonium Assay
• Interferences: U, Np, Fe, and potentially by other metallic elements that have multiple valences
• Alkali metal and alkaline earth metals, Al, Cd, Hf, Zr, Sc and Y do not interfere
• Typically performed using 250 mg sample
• Method can be automated
• Typical precision is 0.05% for an automated method
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Assay by Isotope Dilution Mass Spectrometry
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Assay by Isotope Dilution Mass Spectrometry (cont.)
+
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Isotopic Analysis
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Trace Metal Analysis
• Inductively Coupled Plasma – Atomic Emission Spectroscopy (ICP-AES)
– Primarily use for impurities analysis
– Provides less precise (~10%) measurement for U, Pu or elemental concentrations
– Requires sample dissolution
– Subject to spectral interferences (may require chemical separation)
– Can analyze many elements at one time
– Automated instrumentation
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Trace impurities by ICP-MS
• Sample must be dissolved
– Mass interferences
– Determination of 70 + elements
– Precision typically 5 – 20 %
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Examples of safeguards application
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Age determination using radiochronometers
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DA for IAEA Environmental Safeguards• Environmental safeguards sampling and analysis is a powerful method for
verifying declared operations at safeguarded facilities
• Analyses completed at IAEA Network of World Analytical Laboratories (NWAL)
• Swipe analyses
– NDA gamma spectroscopy
– Uranium assay by ICP-MS or ID TIMS, isotopics by TIMS
– Plutonium assay and isotopics by ID TIMS
• Rigorous QA program
– Process blanks with each set of samples
– Blind QC samples analyzed at least once per year
• Much smaller quantities of material than traditional accountability
– Uranium 1 ng – 10 mg
– Plutonium 1 fg – 10 ng
LANL photo
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NWAL swipe analysis flowsheet
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ICP-MS screening
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Challenges with Environmental Safeguards DA
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Uranium Blanks
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Typical Uranium concentrations in reagents
Reagent
Source: LANL
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Uranium in Anion Resins
Source: LANL
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Uranium in muffle furnaces
Source: LANL
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Environmental Safeguards Summary
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Destructive Analysis Summary
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Acknowledgements
• Uranium blank data and swipe photo were obtained from a LANL presentation “Destructive Analysis Techniques for Safeguards” by Stephen LaMont, Robert Stiener, Lav Tandon, and Paul Mendoza, June 19, 2008
• Photographs of instruments at INL were taken by Jeff Olsen and Mary Adamic