1. 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

2. 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.

3. 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

4. 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.

5. 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 .

6. 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

7. 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.

8. 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.

9. 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

10. 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%

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

12. 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

13. 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

14. 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

15. 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

16. 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

17. 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

18. Recoveries for Direct Spikes

19. Recoveries in DI Water

20. Recoveries in Simulated Hanford Ground Water

21. 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

22. 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