© Copyright, West Valley Nuclear Services Company, LLC (2004) The views expressed by the authors...
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© Copyright, West Valley Nuclear Services Company, LLC (2004) The views expressed by the authors are their own and do not necessarily represent the views of the U.S. Government, the U.S. Department of Energy, the State of New York, or any of its agencies. This document has undergone Export Control Review and has been approved for general release. Iron-55 Analysis on High-Activity Samples with Separation Flow Rates Aided by Vacuum Box Craig Maddigan Analytical & Process Chemistry West Valley Nuclear Services Company
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Transcript of © Copyright, West Valley Nuclear Services Company, LLC (2004) The views expressed by the authors...
© Copyright, West Valley Nuclear Services Company, LLC (2004)
The views expressed by the authors are their own and do not necessarily represent the views of the U.S. Government, the U.S. Department of Energy, the State of New York, or any of its agencies. This document has undergone Export Control Review and has been approved for general release.
Iron-55 Analysis on High-Activity Samples with Separation
Flow Rates Aided by Vacuum Box
Craig MaddiganAnalytical & Process Chemistry
West Valley Nuclear Services Company
© Copyright, West Valley Nuclear Services Company, LLC (2004)
The views expressed by the authors are their own and do not necessarily represent the views of the U.S. Government, the U.S. Department of Energy, the State of New York, or any of its agencies. This document has undergone Export Control Review and has been approved for general release.
Interpreting Statements in Scientific Papers “It has long been known”
– I don’t know the original reference. “3 samples were selected for detailed study”
– Because the other ones STUNK!!! “Additional work will be required to elucidate the
mechanism”– I don’t have a clue what is going on and I am not going
to be the one to figure it out. “Correct within an order of magnitude”
– So very, very wrong.
© Copyright, West Valley Nuclear Services Company, LLC (2004)
The views expressed by the authors are their own and do not necessarily represent the views of the U.S. Government, the U.S. Department of Energy, the State of New York, or any of its agencies. This document has undergone Export Control Review and has been approved for general release.
•Analytical & Process Chemistry Laboratory West Valley Nuclear Services
– Process Support
• Low-Level Wastewater
• Supernatant Treatment (Complete)
• Cement Solidification (Complete)
• Vitrification (Complete)
– Decontamination & Decommissioning
• Plutonium Product Cell
• Extraction Cells
• Head End Cells
© Copyright, West Valley Nuclear Services Company, LLC (2004)
The views expressed by the authors are their own and do not necessarily represent the views of the U.S. Government, the U.S. Department of Energy, the State of New York, or any of its agencies. This document has undergone Export Control Review and has been approved for general release.
•A&PC (contd…) West Valley Nuclear Services
– Waste Characterization• For off-site shipment and disposal
– Facility Characterization• To estimate the Curie count in the facility (post
D&D)
© Copyright, West Valley Nuclear Services Company, LLC (2004)
The views expressed by the authors are their own and do not necessarily represent the views of the U.S. Government, the U.S. Department of Energy, the State of New York, or any of its agencies. This document has undergone Export Control Review and has been approved for general release.
Objectives
Reduce time required to prep samples Reduce analysis waste Increase the accuracy of the analysis by
eliminating interference
© Copyright, West Valley Nuclear Services Company, LLC (2004)
The views expressed by the authors are their own and do not necessarily represent the views of the U.S. Government, the U.S. Department of Energy, the State of New York, or any of its agencies. This document has undergone Export Control Review and has been approved for general release.
Issues/ Areas for Improvement
Laboratory Prep Time was approximately 9 hours per set of samples.
Eu-154 interference required a Chloride column cleanup
Cl- liquids are becoming taboo @ WV due to effect on stainless steel tanks & ventilation
© Copyright, West Valley Nuclear Services Company, LLC (2004)
The views expressed by the authors are their own and do not necessarily represent the views of the U.S. Government, the U.S. Department of Energy, the State of New York, or any of its agencies. This document has undergone Export Control Review and has been approved for general release.
Technician @ Teflon-lined Fume Hood
© Copyright, West Valley Nuclear Services Company, LLC (2004)
The views expressed by the authors are their own and do not necessarily represent the views of the U.S. Government, the U.S. Department of Energy, the State of New York, or any of its agencies. This document has undergone Export Control Review and has been approved for general release.
Old Analysis Scheme for Fe-55
Dissolved samples spiked with elemental Iron & converted to 8 molar nitric acid matrix
Samples were loaded onto an Eichrom TRU column (Gravity)
Column Wash (Gravity) Iron Elution (Europium co-elutes) Convert eluant to 10N HCl
© Copyright, West Valley Nuclear Services Company, LLC (2004)
The views expressed by the authors are their own and do not necessarily represent the views of the U.S. Government, the U.S. Department of Energy, the State of New York, or any of its agencies. This document has undergone Export Control Review and has been approved for general release.
Old Analysis Scheme (contd.) Prep an AG1x8 column as Cl Load sample onto the Cl- column (Gravity) Wash with Cl- (Gravity) Elute with 1 molar nitric Boil down to destroy organics Add to liquid scintillation cocktail or stipple into a conical planchette Dilute for ICP (yield determination) COUNT (LSC or LEPS)
© Copyright, West Valley Nuclear Services Company, LLC (2004)
The views expressed by the authors are their own and do not necessarily represent the views of the U.S. Government, the U.S. Department of Energy, the State of New York, or any of its agencies. This document has undergone Export Control Review and has been approved for general release.
Fe-55 preps and LEPS end cap
© Copyright, West Valley Nuclear Services Company, LLC (2004)
The views expressed by the authors are their own and do not necessarily represent the views of the U.S. Government, the U.S. Department of Energy, the State of New York, or any of its agencies. This document has undergone Export Control Review and has been approved for general release.
Eu-154 interference
Eu-154 is present in spent nuclear fuel and PUREX waste
Eu-154 has an 8% probable photon @6.1KeV
The main Fe-55 photons are @5.9KeV Eu is similar in its chemistry to Am Am (and Eu) are retained on DB in 2M
nitric
© Copyright, West Valley Nuclear Services Company, LLC (2004)
The views expressed by the authors are their own and do not necessarily represent the views of the U.S. Government, the U.S. Department of Energy, the State of New York, or any of its agencies. This document has undergone Export Control Review and has been approved for general release.
New Analysis Scheme for Fe-55 Dissolved Samples spiked with elemental Iron & converted to 8 molar nitric acid matrix Samples loaded on TRU cartridge (Vacuum) Column Wash (Vacuum) Iron Elution is through a DB cartridge, removing Europium (Vacuum) Add to liquid scintillation cocktail or stipple into a conical planchette. COUNT (LSC or LEPS) Dilute for ICP (yield determination)
© Copyright, West Valley Nuclear Services Company, LLC (2004)
The views expressed by the authors are their own and do not necessarily represent the views of the U.S. Government, the U.S. Department of Energy, the State of New York, or any of its agencies. This document has undergone Export Control Review and has been approved for general release.
New Configuration
© Copyright, West Valley Nuclear Services Company, LLC (2004)
The views expressed by the authors are their own and do not necessarily represent the views of the U.S. Government, the U.S. Department of Energy, the State of New York, or any of its agencies. This document has undergone Export Control Review and has been approved for general release.
High-Activity Sample DilutionGeneral Purpose Cell Log#03-0598 EXAMPLE dilution alpha-beta 10.2112 g of sample 226.623 g dilution 1 1.0145 g of dilution 1 243.5632 g dilution 2 10.5831 g of dilution 2 is matrix converted Cl- to
nitric 12.0826 g of matrix converted “dilution 3” 0.1213 g taken for gross alpha-beta
© Copyright, West Valley Nuclear Services Company, LLC (2004)
The views expressed by the authors are their own and do not necessarily represent the views of the U.S. Government, the U.S. Department of Energy, the State of New York, or any of its agencies. This document has undergone Export Control Review and has been approved for general release.
High-Activity Sample Results
General Purpose Cell Log #03-0598 Gross Alpha 1.76E+0 uCi/g Gross Beta 2.01E+2 Am-241 1.03E+0 Cs-137 6.35E+0 Alpha Pu 9.10E-1 Sr-90 4.87E+0 Fe-55 2.10E+1 Co-60 1.24E+2 Eu-154 2.53E-2
© Copyright, West Valley Nuclear Services Company, LLC (2004)
The views expressed by the authors are their own and do not necessarily represent the views of the U.S. Government, the U.S. Department of Energy, the State of New York, or any of its agencies. This document has undergone Export Control Review and has been approved for general release.
Laboratory Test Procedure 030791
Laboratory Test Procedure 030791
uCi/g or uCi/mL
General Purpose Cell
03-0598 QC1 QC2 QC3 QC4 QC5 QC6
Original 21.5 2.10E-03 2.10E-03 2.10E-03 2.10E-03 2.10E-03 2.10E-03 Ave/True
Fe-LEPS 2.33E+01 2.26E-03 2.49E-03 2.38E-03 2.37E-03 2.02E-03 1.87E-03 QC AVE 2.23E-03 1.06Fe-LSC 1.99E+01 1.94E-03 2.01E-03 2.00E-03 1.95E-03 2.05E-03 1.88E-03 QC AVE 1.97E-03 0.94
QC TRUE 2.10E-03
% difference
LEPS 8.4 7.6 18.6 13.3 12.9 -3.8 -11.0
LSC -7.4 -7.6 -4.3 -4.8 -7.1 -2.4 -10.5
