Radioactive Materials Analytical Laboratory Eichrom Technologies Eichrom Technologies Inc. User Group Inc. User Group Meeting May 2001 Meeting May 2001 J.M. Giaquinto , L.D. Bible, D.C. Glasgow, J.M. Keller Chemical and Analytical Sciences Division Oak Ridge National Laboratory
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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 - PowerPoint PPT Presentation
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Radioactive Materials Analytical Laboratory
Eichrom Technologies Inc. User Eichrom Technologies Inc. User Group Meeting May 2001Group Meeting May 2001
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
Project: Project: Trace Actinides in Nickel MetalTrace Actinides in Nickel Metal
DOE metals reclamation projectLimited funding21 day turnaround
Radioactive Materials Analytical Laboratory
Project: Project: Trace Actinides in Nickel MetalTrace 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
Project: Project: Trace Actinides in Nickel MetalTrace Actinides in Nickel Metal
Reduction of Np– 5mL digestate– 2mL 1M hydroxylamine– Heat between 80C to 100C for
1hr
Radioactive Materials Analytical Laboratory
Project: Project: Trace Actinides in Nickel MetalTrace 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
Project: Project: Trace Actinides in Nickel MetalTrace 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
Project: Project: Trace Actinides in Nickel MetalTrace Actinides in Nickel Metal
20%30%40%50%60%70%80%90%
100%110%120%130%
Percent Recovery
Th-232 83% 73% 99% 90% 120%
U-233 76% 74% 49% 97% 93% 91% 96%
Np237 93% 92% 36% 75% 93% 90% 97%
Pu-242 101% 99% 46% 81% 100% 99% 102%
1 2 33 re-prep
4 5 6
MatrixSpike Recoveries
Radioactive Materials Analytical Laboratory
Project: Project: Trace Level Gallium Analysis in MOX Trace Level Gallium Analysis in MOX Fuels (Irradiated and Un-Irradiated)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
Radioactive Materials Analytical Laboratory
Radioactive Materials Analytical Laboratory
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
Radioactive Materials Analytical Laboratory
Project: Project: Trace Level Gallium Analysis in MOX Trace Level Gallium Analysis in MOX Fuels (Irradiated and Un-Irradiated)Fuels (Irradiated and Un-Irradiated)
MatrixSpike Recoveries
20%
30%
40%
50%
60%
70%
80%
90%
100%
110%
120%
130%
Percent Recovery
Ga 96% 95% 94% 92% 92% 91% 107%
1 2 3 4 5 6 7
Radioactive Materials Analytical Laboratory
Project: Project: Baseline Separation of High Mass Fission Baseline Separation of High Mass Fission Products (REEs) For Burn-up CalculationsProducts (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
Project: Project: Baseline Separation of High Mass Fission Baseline Separation of High Mass Fission Products (REEs) For Burn-up CalculationsProducts (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
Radioactive Materials Analytical Laboratory
Project: Project: Baseline Separation of High Mass Fission Baseline Separation of High Mass Fission Products (REEs) For Burn-up CalculationsProducts (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
Baseline separation of Ce, Nd, and Sm Using Eichrom LN Resin