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The Determination Of 226 Ra In Soil Samples

The Determination Of 226 Ra In Soil Samples. Lawrence D. Morris General Engineering Laboratories, Inc. Anil H. Thakkar Eichrom Technologies, Inc. Objective: Design a reliable method to measure 226 Ra in soil samples by Alpha Spectroscopy thus meeting the current need of our clients.

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The Determination Of 226 Ra In Soil Samples

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  1. The Determination Of 226RaIn Soil Samples Lawrence D. Morris General Engineering Laboratories, Inc. Anil H. Thakkar Eichrom Technologies, Inc.

  2. Objective: Design a reliable method to measure 226Ra in soil samples by Alpha Spectroscopy thus meeting the current need of our clients. • Faster Turn Around Times than current methods • This procedure utilizes Cation and Eichrom’s Ln Resin • Achieve Peak Resolution (FWHM) of less than 100keV General Engineering Laboratories, Inc. Charleston, SC

  3. Anil Thakkar visited GEL in April • Discussed the Radium in Water procedure • Ran some test samples General Engineering Laboratories, Inc. Charleston, SC

  4. Spectrum from Testing Water Procedure General Engineering Laboratories, Inc. Charleston, SC

  5. Spectrum from Testing Water Procedure • This brought up the question about how well the procedure would work with soils? General Engineering Laboratories, Inc. Charleston, SC

  6. Highlights of the Procedure:Radium in Water (RAW03)Eichrom Technologies, Inc. • Digest the sample • Dissolve the residue with dilute HNO3 • Pass sample through Cation resin column • Elute Ra and Ba with 8M HNO3 • Evaporate eluate to dryness • Dissolve residue with 0.095M HNO3 General Engineering Laboratories, Inc. Charleston, SC

  7. Highlights of the Procedure:Radium in Water (RAW03)Eichrom Technologies, Inc. • Pass through Ln Column collecting the eluate for determination of 226Ra • Perform Barium Sulfate micro-precipitation • Filter • Count on Gamma for Tracer Recovery (133Ba) • Count on Alpha for 226Ra determination General Engineering Laboratories, Inc. Charleston, SC

  8. Test #1 Results General Engineering Laboratories, Inc. Charleston, SC

  9. Test #1 SpectraSample 1 General Engineering Laboratories, Inc. Charleston, SC

  10. Test #1 SpectraSample 3 General Engineering Laboratories, Inc. Charleston, SC

  11. Test #1 SpectraSample 6 (LCS) General Engineering Laboratories, Inc. Charleston, SC

  12. Problem with initial testing: • Resolution exceeded 100keV • Suspected cause was from natural Barium in the soil. General Engineering Laboratories, Inc. Charleston, SC

  13. Proposed solutions: • Use less sample • Use less Barium Carrier • 100L of 0.75 mg/mL Barium Carrier was used for Test #1 • Use less Seeding Suspension General Engineering Laboratories, Inc. Charleston, SC

  14. Test #2 • Analyze 3 samples with No Barium Carrier • Analyze 3 samples with 50 L of Barium Carrier • Vary aliquot size from 0.1g to 0.5g General Engineering Laboratories, Inc. Charleston, SC

  15. Test #2 Results General Engineering Laboratories, Inc. Charleston, SC

  16. Problem with Test #2: • Resolution on samples with reduced Barium Carrier continue to exceed 100keV General Engineering Laboratories, Inc. Charleston, SC

  17. Test #2 SpectraSample 1 General Engineering Laboratories, Inc. Charleston, SC

  18. Test #2 SpectraSample 3 General Engineering Laboratories, Inc. Charleston, SC

  19. Test #3 • Used 0.1mL of the seeding suspension • 0.2mL used previously • No Barium Carrier was used General Engineering Laboratories, Inc. Charleston, SC

  20. No Barium Yields FAILURE Test #3 General Engineering Laboratories, Inc. Charleston, SC

  21. Test #4 • Comparison of Alpha Spec vs. Emanation • Alpha Spec • Used 0.2g of sample • 50L of Barium Carrier • Emanation used 0.5g of sample General Engineering Laboratories, Inc. Charleston, SC

  22. Test #4 Results General Engineering Laboratories, Inc. Charleston, SC

  23. Test #4 SpectraSample 1 General Engineering Laboratories, Inc. Charleston, SC

  24. Test #4 SpectraSample 2 General Engineering Laboratories, Inc. Charleston, SC

  25. Update to the Objective • Further discussions with the client revealed they were never able to achieve resolution <100keV • They re-set their requirement to <250keV • Current testing Average FWHM • 149keV • Consistently <200keV General Engineering Laboratories, Inc. Charleston, SC

  26. Changes to 226Ra Water Procedure • Ensure that 0.5g or less of soil used • Minimizes natural Barium introduced • Reduce Barium carrier used • 50µL 0.75mg/mL General Engineering Laboratories, Inc. Charleston, SC

  27. In Conclusion • Original FWHM Goal (<100keV) not achieved • Client changed their requirement to <250keV • Average FWHM for soils 149keV • Faster Turn Around Times accomplished • Soils can be run in 2 days • Emanation 3 day minimum • Gamma 7-30 day minimum • Waters can be run in 1 day General Engineering Laboratories, Inc. Charleston, SC

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