A Rapid Analysis of Actinides In Urine Samples

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

Current Eichrom Method • UTEVA and TRU Resin Column • Industry Standard • Flow Rate Limitation

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

Tandem Column Arrangement Load U T T R E U V Discard Strip A Strip U Pu Am

Eichrom UTEVA Resin Column Separation Load: 3 M HNO 3, 1. 0 M Al(NO 3)3 0. 01 M HCl to TRU Resin column U

Eichrom TRU Resin Column Separation Load: 3 M HNO 3, 1. 0 M Al(NO 3)3 to waste 9 m HCl & 4 M HCl Am 0. 1 M ammonium bioxalate Pu

Decontamination Factors (DF) • To determine the ruggedness of the method • To determine the degree of separation of the analyte from potentially interfering matrix components

Experiment for DF • Approximately 100 p. Ci (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

Criteria for Acceptance • For actinides, a DF value of > 1000 is acceptable • Tracer Recovery: 70%-105%

Decontamination Factors (with column)

New Configuration: Resin Cartridge • Packed with 2 m. L of resin • Cartridges with Luer lock • Ease of tandem arrangement for sequential analysis

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 m. L C Tubes • Eichrom has limited stock on hand

Decontamination Factors (with Cartridge)

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 Ca 3(PO 4)2 precipitation was performed • Decant supernatant, centrifuge and collect the precipitate • Perform a wet digestion on the precipitate until white ash

Load Solution for UTEVA and TRU Resin Columns • Dissolve precipitate in 3 M HNO 3/1 M Al(NO 3)3 solution • Add ferrous sulfamate and ascorbic acid • Load on UTEVA and TRU Resin cartridge in tandem

Am/Cm, Pu and U Analyses Calcium phosphate precipitation Wet ash digestion Eichrom U/TEVA Resin Eichrom TRU Resin Preparation for counting Alpha spectrometry U Am/Cm, Pu

Flow rate • Sample load: Typically 1 m. L/minute • Rinse solution: 2 -3 m. L/minute • Strip solution: 1 m. L/minute • Achievable with vacuum pump

Recoveries for Direct Spikes

Recoveries in DI Water

Recoveries in Simulated Hanford Ground Water

Recoveries in Synthetic Urine Samples

Recoveries in Real Urine Samples

PROCORAD French Intercomparison Samples

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

Eichrom Cartridges • • Available in TRU, TEVA, UTEVA and Sr Other Resins available by special order 2 m. L 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

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