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

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Tandem Column Arrangement

Discard

TRUUTEVA

Strip

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

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

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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

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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

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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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Flow rate

• Typically 2-3 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)

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

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