1 / 32

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

A Rapid Analysis of Actinides In Urine Samples Using Eichrom’s Resin Cartridges. Anil H.Thakkar Eichrom Industries, Inc.. Darien, IL. Objective. To perform analysis for Am, Pu and U in urine samples using Eichrom’s new chromatographic configuration of UTEVA and TRU Resin.

kirsi
Download Presentation

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

An Image/Link below is provided (as is) to download presentation Download Policy: Content on the Website is provided to you AS IS for your information and personal use and may not be sold / licensed / shared on other websites without getting consent from its author. Content is provided to you AS IS for your information and personal use only. Download presentation by click this link. While downloading, if for some reason you are not able to download a presentation, the publisher may have deleted the file from their server. During download, if you can't get a presentation, the file might be deleted by the publisher.

E N D

Presentation Transcript


  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

  24. Recoveries in Real Urine Samples

  25. PROCORADFrench Intercomparison Samples

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

  27. 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

  28. 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

More Related