1. © 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

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. Interpreting Statements in Scientific Papers 4 “It has long been known” –I don’t know the original reference. 4 “3 samples were selected for detailed study” –Because the other ones STUNK!!! 4 “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. 4 “Correct within an order of magnitude” –So very, very wrong.

3. © 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 4 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

4. © 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…) 4 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)

5. © 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 4 Reduce time required to prep samples 4 Reduce analysis waste 4 Increase the accuracy of the analysis by eliminating interference

6. © 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 4 Laboratory Prep Time was approximately 9 hours per set of samples. 4 Eu-154 interference required a Chloride column cleanup 4 Cl- liquids are becoming taboo @ WV due to effect on stainless steel tanks & ventilation

7. © 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

8. © 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 4 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) K Convert eluant to 10N HCl

9. © 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.) K Prep an AG1x8 column as Cl  Load sample onto the Cl- column (Gravity)  Wash with Cl- (Gravity)  Elute with 1 molar nitric K Boil down to destroy organics 4 Add to liquid scintillation cocktail or stipple into a conical planchette 4 Dilute for ICP (yield determination) 4 COUNT (LSC or LEPS)

10. © 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

11. © 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 4 Eu-154 is present in spent nuclear fuel and PUREX waste 4 Eu-154 has an 8% probable photon @6.1KeV 4 The main Fe-55 photons are @5.9KeV 4 Eu is similar in its chemistry to Am 4 Am (and Eu) are retained on DB in 2M nitric

12. © 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 4 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) 4 Add to liquid scintillation cocktail or stipple into a conical planchette. 4 COUNT (LSC or LEPS) 4 Dilute for ICP (yield determination)

13. © 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

14. © 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 Dilution General Purpose Cell Log#03-0598 4 EXAMPLE dilution alpha-beta 4 10.2112g of sample 4 226.623g dilution 1 4 1.0145g of dilution 1 4 243.5632g dilution 2 4 10.5831g of dilution 2 is matrix converted Cl - to nitric 4 12.0826g of matrix converted “dilution 3” 4 0.1213g taken for gross alpha-beta

15. © 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 4 General Purpose Cell Log #03-0598 4 Gross Alpha1.76E+0uCi/g 4 Gross Beta2.01E+2 4 Am-2411.03E+0 4 Cs-1376.35E+0 4 Alpha Pu9.10E-1 4 Sr-904.87E+0 4 Fe-552.10E+1 4 Co-601.24E+2 4 Eu-1542.53E-2

16. © 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