A Rapid Analysis of Actinides In Urine Samples Using Eichroms Resin Cartridges

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A Rapid Analysis of Actinides In Urine Samples
Using Eichroms Resin Cartridges

• Anil H.Thakkar
• Eichrom Industries, Inc..
• Darien, IL

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Objective

• To perform analysis for Am, Pu and U in urine
  samples using Eichroms new chromatographic
  configuration of UTEVA and TRU Resin

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Current Eichrom Method

• UTEVA and TRU Resin Column
• Industry Standard
• Flow Rate Limitation

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Precedent Actinides in Water

• 1 liter water samples
• Coprecipitate with calcium phosphate
• Dissolve in load solution
• Load on UTEVA and TRU columns in tandem

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Tandem Column Arrangement
Load
Discard
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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
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Decontamination Factors (DF)

• To determine the ruggedness of the method
• To determine the degree of separation of the
  analyte from potentially interfering matrix
  components

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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.

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Equation for Decontamination Factor

• DF Ao
• Af
• Where
• Ao Original activity of the analyte added
  
• Af Final activity of analyte in the fraction

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Criteria for Acceptance

• For actinides, a DF value of gt 1000 is
  acceptable
• Tracer Recovery 70-105

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Decontamination Factors (with column)
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New ConfigurationResin Cartridge

• Packed with 2 mL of resin
• Cartridges with Luer lock
• Ease of tandem arrangement for sequential
  analysis

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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

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Decontamination Factors (with Cartridge)
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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

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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

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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
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Flow rate

• Sample load Typically 1 mL/minute
• Rinse solution 2-3 mL/minute
• Strip solution 1 mL/minute
• Achievable with vacuum pump

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Recoveries for Direct Spikes
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Recoveries in DI Water
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Recoveries in Simulated Hanford Ground Water
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Recoveries in Synthetic Urine Samples
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Recoveries in Real Urine Samples
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PROCORADFrench Intercomparison Samples
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Summary

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

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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

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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