a rapid analysis of actinides in water samples using eichrom’s resin cartridges
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A Rapid Analysis of Actinides In Water Samples Using
Eichrom’s Resin Cartridges Anil H.Thakkar
Eichrom Industries, Inc..
Darien, IL
EIChroMI N D U S T R I E S , I N C.
Objective
• To perform analysis for Am, Pu and U in water samples using Eichrom’s new chromatographic configuration of UTEVA and TRU Resin
EIChroMI N D U S T R I E S , I N C.
Current Eichrom Method
• UTEVA and TRU Resin Column
• Industry Standard
• Flow Rate Limitation
EIChroMI N D U S T R I E S , I N C.
Tandem Column Arrangement
Discard
TRUUTEVA
Strip
Strip
PuU
Am
Load
EIChroMI N D U S T R I E S , I N C.
Eichrom UTEVA Resin Column Separation
Load: 3M HNO3, 1.0M Al(NO3)3
0.01M HCl
to TRU Resin column
U
EIChroMI N D U S T R I E S , I N C.
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
EIChroMI N D U S T R I E S , I N C.
Decontamination Factors (DF)
• To determine the ruggedness of the method
• To determine the degree of separation of the analyte from potentially interfering matrix components
EIChroMI N D U S T R I E S , I N C.
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.
Equation for Decontamination Factor
DF = Ao
Af
Where;
Ao = Original activity of the analyte added
Af = Final activity of analyte in the fraction
EIChroMI N D U S T R I E S , I N C.
Criteria for Acceptance
• For actinides, a DF value of > 1000 is acceptable
• Tracer Recovery: 70%-105%
EIChroMI N D U S T R I E S , I N C.
Decontamination Factors
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
EIChroMI N D U S T R I E S , I N C.
New Configuration:Resin Cartridge
• Packed with 0.7 gram of resin
• Cartridges with Luer lock
• Ease of tandem arrangement for sequential analysis
EIChroMI N D U S T R I E S , I N C.
Testing the procedure with Cartridges
• 1 liter aliquots of sample were spiked with Am, Pu, and U
EIChroMI N D U S T R I E S , I N C.
Am/Cm, Pu and U AnalysesCalcium phosphate precipitation
Dissolve in load solution
Eichrom U/TEVA Resin U
Eichrom TRU Resin Am/Cm, Pu
Preparation for counting
Alpha spectrometry
EIChroMI N D U S T R I E S , I N C.
Sample Preparation
• l liter aliquots of acidified water samples were spiked with Am, Pu and U
• Samples were heated to near boiling for at least 3 hours
• A Ca3(PO4)2 precipitation was performed
• Decant supernatant, centrifuge and collect the precipitate
EIChroMI N D U S T R I E S , I N C.
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
EIChroMI N D U S T R I E S , I N C.
Flow rate
• Typically 2-3 mL/minute
• Achievable with vacuum pump
EIChroMI N D U S T R I E S , I N C.
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)
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)
Recoveries in Simulated Hanford Ground Water
Actinide Column Cartridge
Am 92% 79+8% (n=4)
U 84% 78+9% (n=4)
Pu 96% 82+4% (n=4)
Summary
• Eichrom Resin cartridges provide fast separation for actinides
• Good, reproducible and consistent recoveries achievable
• Rapid turn-around possible
EIChroMI N D U S T R I E S , I N C.
Future Objectives
• Evaluate effect of flow rate on chemical recovery
• To test other matrices such as; urine, soil and vegetation for actinides using Eichrom Resin cartridges
• To evaluate separation of Sr using Eichrom Sr Resin cartridges
EIChroMI N D U S T R I E S , I N C.
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