Anil H.Thakkar Eichrom Industries, Inc.. Darien, IL A Rapid Analysis of Actinides In Water Samples Using Eichrom’s Resin Cartridges Anil H.Thakkar Eichrom Industries, Inc.. Darien, IL In response to to our industry needs for a suitable procedure for am, pu & U in urine samples, eichrom has devpd. a method using eichrom’s extraction chromatographic resins. In this talk I will discuss the method & the results for tracer recoveries in real & synthetic urine samples

EIChroM I 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 An improved procedure was developed to separate Am,Pu and U in variety of water matrices.

Current Eichrom Method I 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

Tandem Column Arrangement EIChroM I N D U S T R I E S , I N C. Tandem Column Arrangement TRU UTEVA Strip Pu U Am Load Discard Load soln. is passed thru Uteva first, followed by TRu. U is reomoved on UTeva, while Am & Pu on TRU.

Eichrom UTEVA Resin Column Separation I 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 On Uteva spec, the actinides were loaded with a load solution of 3M HNO3/1.0 M Al(NO3)3 solution, Pu+4 was reduce by Iron Pu+3. U gets stuck on Uteva, while PU & Am passes thru the column Am/Pu pass thru, Uteva, therefore the load solution and rinse are collected, Uranium is stripped by 0.01 M HCl .

Eichrom TRU Resin Column Separation I 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 to waste 9m HCl & 4M HCl Am The eluants from Uteva are loaded on to Tru column. Am is stripped using 9M Hcl & 4M HCl. Pu with 0.1 M Am. Bioxalate. 0.1M ammonium bioxalate Pu

Decontamination Factors (DF) EIChroM I 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 The other imp. aspect of this proposal was to look at the Decontamination of possible interfering actinides in this procedure. Also to check the ruggedness and to see if clean separation was achieved for the actinides of interest.

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 EIChroM I N D U S T R I E S , I N C. 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 EIChroM I 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%

Decontamination Factors EIChroM I N D U S T R I E S , I N C. Decontamination Factors

New Configuration:Resin Cartridge EIChroM I 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

Testing the procedure with Cartridges EIChroM I 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

Am/Cm, Pu and U Analyses EIChroM Calcium phosphate precipitation I N D U S T R I E S , I N C. Am/Cm, Pu and U Analyses Calcium phosphate precipitation Dissolve in load solution Eichrom U/TEVA Resin U Eichrom TRU Resin Am/Cm, Pu Preparation for counting Alpha spectrometry

EIChroM I 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

Load Solution for UTEVA and TRU Resin Columns EIChroM I 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

Flow rate Typically 2-3 mL/minute Achievable with vacuum pump EIChroM I N D U S T R I E S , I N C. Flow rate Typically 2-3 mL/minute Achievable with vacuum pump

Recoveries for Direct Spikes

Recoveries in DI Water

Recoveries in Simulated Hanford Ground Water

Summary Eichrom Resin cartridges provide fast separation for actinides I N D U S T R I E S , I N C. Summary Eichrom Resin cartridges provide fast separation for actinides Good, reproducible and consistent recoveries achievable Rapid turn-around possible

Future Objectives Evaluate effect of flow rate on chemical recovery EIChroM I 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