A Rapid Analysis of Actinides In Urine Samples Using Eichrom’s Resin Cartridges

1. A Rapid Analysis of Actinides In Urine Samples Using Eichrom’s Resin Cartridges Anil H.Thakkar Eichrom Industries, Inc.. Darien, IL

2. Objective • To perform analysis for Am, Pu and U in urine samples using Eichrom’s new chromatographic configuration of UTEVA and TRU Resin

3. CurrentEichrom Method • UTEVA and TRU Resin Column • Industry Standard • Flow Rate Limitation

4. Precedent: Actinides in Water • 1 liter water samples • Coprecipitate with calcium phosphate • Dissolve in load solution • Load on UTEVA and TRU columns in tandem

5. U T E V A T R U Strip Strip U Pu Am Tandem Column Arrangement Load Discard

6. Eichrom UTEVA Resin Column Separation Load: 3M HNO3, 1.0M Al(NO3)3 to TRU Resin column 0.01M HCl U

7. Eichrom TRU Resin Column Separation Load: 3 M HNO3, 1.0M Al(NO3)3 to waste 9m HCl & 4M HCl Am 0.1M ammonium bioxalate Pu

8. Decontamination Factors (DF) • To determine the ruggedness of the method • To determine the degree of separation of the analyte from potentially interfering matrix components

9. Experiment for DF • Approximately 100 pCi (3.7 Bq) of each actinide was added to a load solution and run through the method. • DF in uranium, plutonium and americium fractions were calculated.

10. Equation for Decontamination Factor DF = Ao Af Where; Ao = Original activity of the analyte added Af = Final activity of analyte in the fraction

11. Criteria for Acceptance • For actinides, a DF value of > 1000 is acceptable • Tracer Recovery: 70%-105%

12. Decontamination Factors (with column)

13. New Configuration:Resin Cartridge • Packed with 2 mL of resin • Cartridges with Luer lock • Ease of tandem arrangement for sequential analysis

14. Eichrom Vacuum Box System • 24 Hole clear polycarbonate vacuum box • Inexpensive cartridge connection • Yellow outer tip provides support • White inner tip provides excellent seal • Vacuum gauge • Plastic rack for twenty four 50 mL C Tubes • Eichrom has limited stock on hand

15. Decontamination Factors (with Cartridge)

16. Sample Preparation • 1.2 liter aliquots of acidified urine samples were spiked with Am, Pu and U • Samples were heated to near boiling for 2 hours • A Ca3(PO4)2 precipitation was performed • Decant supernatant, centrifuge and collect the precipitate • Perform a wet digestion on the precipitate until white ash

17. Load Solution for UTEVA and TRU Resin Columns • Dissolve precipitate in 3M HNO3/1M Al(NO3)3 solution • Add ferrous sulfamate and ascorbic acid • Load on UTEVA and TRU Resin cartridge in tandem

18. Am/Cm, Pu and U Analyses Calcium phosphate precipitation Wet ash digestion Eichrom U/TEVA Resin U Eichrom TRU Resin Am/Cm, Pu Preparation for counting Alpha spectrometry

19. Flow rate • Sample load: Typically 1 mL/minute • Rinse solution: 2-3 mL/minute • Strip solution: 1 mL/minute • Achievable with vacuum pump

20. Recoveries for Direct Spikes

21. Recoveries in DI Water

22. Recoveries in Simulated Hanford Ground Water

23. Recoveries in Synthetic Urine Samples

25. Recoveries in Real Urine Samples

28. PROCORADFrench Intercomparison Samples

30. Summary • Eichrom Resin cartridges provide fast separation for actinides • Good, reproducible and consistent recoveries achievable • Rapid turn-around possible

31. Eichrom Cartridges • Available in TRU, TEVA, UTEVA and Sr • Other Resins available by special order • 2 mL Resin volume • Standard S grade, 50-100 micron beads • Can be stacked using Luer connections • Standard syringe barrel used for reservoir • Individually labeled w/ lot number

32. Future Objectives • Evaluate effect of faster flow rate on chemical recovery • To test other matrices such as; fecal, soil and vegetation for actinides using Eichrom Resin cartridges • To evaluate separation of Sr using Eichrom Sr Resin cartridges