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Eichrom Technologies Inc. User Group Meeting May 2001

Eichrom Technologies Inc. User Group Meeting May 2001. J.M. Giaquinto , L.D. Bible, D.C. Glasgow, J.M. Keller Chemical and Analytical Sciences Division Oak Ridge National Laboratory. Projects To Be Discussed. Trace level actinides analysis in nickel metal

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Eichrom Technologies Inc. User Group Meeting May 2001

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  1. Eichrom Technologies Inc. User Group Meeting May 2001 J.M. Giaquinto, L.D. Bible, D.C. Glasgow, J.M. Keller Chemical and Analytical Sciences Division Oak Ridge National Laboratory Radioactive Materials Analytical Laboratory

  2. Projects To Be Discussed • Trace level actinides analysis in nickel metal • Trace level gallium analysis in mixed oxide fuels (irradiated and un-irradiated) • Baseline separation of high mass fission products (REEs) for burn-up analysis and calculation • Trace level iridium analysis in ancient bone fragments by NAA Radioactive Materials Analytical Laboratory

  3. Project: Trace Actinides in Nickel Metal • DOE metals reclamation project • Limited funding • 21 day turnaround Radioactive Materials Analytical Laboratory

  4. Project: Trace Actinides in Nickel Metal • 65% Nickel • 30% Copper • 2% Iron • 6.5 M HNO3 • To meet project reporting limits only a max. 20-fold dilution allowed Radioactive Materials Analytical Laboratory

  5. Project: Trace Actinides in Nickel Metal • Reduction of Np • 5mL digestate • 2mL 1M hydroxylamine • Heat between 80C to 100C for 1hr Radioactive Materials Analytical Laboratory

  6. Project: Trace Actinides in Nickel Metal • Sample loading • Let solution cool • Build to ~7 mL with distilled water • Load onto pre-conditioned TRU Resin • 1 to 2 mL/min flow • Rinse with 5 mL of 4 M HNO3 Radioactive Materials Analytical Laboratory

  7. Project: Trace Actinides in Nickel Metal • Sample elution • Elute with 10 mL of 0.1 M oxalate in 0.005 M HNO3 • 1 to 2 mL/min flow • Matrix adjustment • Heat eluant at 100C to 150C until volume reduced to ~2 mL • Destroy oxalate • Cool and collect solution. Build to 5 mL with 0.5 M HNO3 • Ready for ICPMS analysis Radioactive Materials Analytical Laboratory

  8. Project: Trace Actinides in Nickel Metal Matrix Spike Recoveries Radioactive Materials Analytical Laboratory

  9. Project: Trace Level Gallium Analysis in MOX Fuels (Irradiated and Un-Irradiated) • Analysis performed at the request of the Fissile Materials Disposition Program (FMDP) • Gallium mixed with the plutonium product • Reporting limits in the 10’s of ppb required for the un-irradiated enriched uranium product Radioactive Materials Analytical Laboratory

  10. Radioactive Materials Analytical Laboratory

  11. Radioactive Materials Analytical Laboratory

  12. TRU Resin Separation-Sample digestion matrix adjusted to 2.5 M to 4.0 M nitric acid. -5 mL portion passed through column conditioned with 2.5 M nitric acid. Elution collected. - Column rinsed with 5 mL 2.5 M nitric acid. Rinse collected with earlier eluant - Volume adjusted if needed. Ready for ICP-MS analysis Radioactive Materials Analytical Laboratory

  13. Radioactive Materials Analytical Laboratory

  14. Project: Trace Level Gallium Analysis in MOX Fuels (Irradiated and Un-Irradiated) Matrix Spike Recoveries Radioactive Materials Analytical Laboratory

  15. Project: Baseline Separation of High Mass Fission Products (REEs) For Burn-up Calculations • Analysis performed at the request of the Fissile Materials Disposition Program (FMDP) • ASTM E 321-96 Standard Test Method for Atom Percent Fission in Uranium and Plutonium Fuel (Nd-148 Method) Radioactive Materials Analytical Laboratory

  16. Project: Baseline Separation of High Mass Fission Products (REEs) For Burn-up Calculations • Uranium and Plutonium fractions are separated using Anion Exchange Resin • Neodymium fraction • ASTM separation • Time consuming • Multiple reagents • Eichrom Ln Resin • Simple separation scheme • One reagent (0.18 M HCL) • Can re-use column once it is calibrated Radioactive Materials Analytical Laboratory

  17. Radioactive Materials Analytical Laboratory

  18. Project: Baseline Separation of High Mass Fission Products (REEs) For Burn-up Calculations Ln Resin Separation - 5 mL to 6 mL bed volume - Resin conditioned with 0.18 M HCl - Sample matrix adjusted to 0.18 M HCl - Sample loaded onto column and rinsed through with 0.18 M HCl. Eluant collected in 5 mL fractions. - Nd fractions combined and dried for TIMS analysis Radioactive Materials Analytical Laboratory

  19. Radioactive Materials Analytical Laboratory

  20. Project: Trace Level Iridium Analysis In Ancient Bone Fragments By NAA • Cretaceous-Tertiary (K/T) geological boundary is defined by an excessive deposit of iridium • Typically iridium present at ultra-trace (<100ppt) levels in materials of geological interest • Separation needed to isolate and concentrate Ir for NAA Radioactive Materials Analytical Laboratory

  21. Project: Trace Level Iridium Analysis In Ancient Bone Fragments By NAA Neutron Activation Analysis for Iridium 191Ir 192Ir (n,gamma) gamma 316 KeV T 1/2=74 days 193Ir 194Ir (n,gamma) gamma 328 KeV T 1/2=19 hrs Radioactive Materials Analytical Laboratory

  22. Project: Trace Level Iridium Analysis In Ancient Bone Fragments By NAA Established separation schemes are elaborate, time consuming and more prone to yield reduction Radioactive Materials Analytical Laboratory

  23. Project: Trace Level Iridium Analysis In Ancient Bone Fragments By NAA • TEVA Separation: • Load sample digestion (8 M HNO3/6 M HCl) onto column treated with 2 M HNO3 • Pass through with vacuum • Wash with 2.5 mL of 2 M HNO3 • Dry and seal column for neutron activation Radioactive Materials Analytical Laboratory

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