a rapid analysis of actinides in urine samples using eichrom’s resin cartridges
DESCRIPTION
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. - PowerPoint PPT PresentationTRANSCRIPT
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A Rapid Analysis of Actinides In Urine Samples Using
Eichrom’s 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 Eichrom’s 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
Discard
T
R
U
U
T
E
V
AStrip
Strip
PuU
Am
Load
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Eichrom UTEVA Resin Column Separation
Load: 3M HNO3, 1.0M Al(NO3)3
0.01M HCl
to TRU Resin column
U
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Eichrom TRU Resin Column Separation
Load: 3 M HNO3, 1.0M Al(NO3)3
9m HCl & 4M HCl
0.1M ammonium bioxalate
to waste
Am
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 > 1000 is acceptable
• Tracer Recovery: 70%-105%
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Decontamination Factors (with column)
Actinide DF in U fraction
DF in Pu fraction
DF in Am fraction
U-232 N/A 3300->5600 900->4000
Pu-242 1200-1400 N/A >2400
Am-243 1400->4300 1600 N/A
Th-228 2800-3300 3400-4000 >3600
Np-237 1100-1200 3500->3900 >3900
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New Configuration:Resin 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)
Actinide DF in U fraction
DF in Pu fraction
DF in Am fraction
U-232 N/A 7300 >5800
Pu-239/240 12,000 N/A 7000
Am-241 >6600 20,000 N/A
Th-229 15,000 10,000 >10,000
Np-237 3500 7000 >12,000
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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 AnalysesCalcium 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
Actinide Column Cartridge
Am 88% 75+12%(n=4)
U 100% 89+6% (n=4)
Pu 83% 92+8% (n=4)
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Recoveries in DI Water
Actinide Column Cartridge
Am 72+13% (n=8) 84+6% (n=4)
U 90+2% (n=8) 84+9% (n=4)
Pu 96+2% (n=4) 70+5% (n=4)
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Recoveries in Simulated Hanford Ground Water
Actinide Column Cartridge
Am 92% 79+8%
U 84% 78+9%
Pu 96% 82+4%
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Recoveries in Synthetic Urine Samples
Actinide Column Cartridge
Am 72 + 13% 76 + 9%
U 89 + 6% 98 + 3%
Pu 96 + 2% 80 + 6%
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Recoveries in Real Urine Samples
Actinide Column Cartridge
Am 75 + 8% 72 + 11%
U 82 + 9% 83 + 6%
Pu 94 + 4% 95 + 6%
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PROCORADFrench Intercomparison SamplesSample U-234
dpm/LU-232(tracer)
1 2.94 + 0.38 79 %
2 2.79 + 0.31 89 %
3 2.66 + 0.33 83 %
Procoradvalue
2.81+ 0.28
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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