Technical Updates on UTEVA, TEVA and TRU Resins Anil Thakkar & Michael Fern Eichrom Technologies,...
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Transcript of Technical Updates on UTEVA, TEVA and TRU Resins Anil Thakkar & Michael Fern Eichrom Technologies,...
![Page 1: Technical Updates on UTEVA, TEVA and TRU Resins Anil Thakkar & Michael Fern Eichrom Technologies, Inc. Paris May 14, 2002.](https://reader035.fdocuments.in/reader035/viewer/2022062313/56649d0a5503460f949dc4c6/html5/thumbnails/1.jpg)
Technical Updates on UTEVA, TEVA and TRU Resins
Anil Thakkar & Michael Fern
Eichrom Technologies, Inc.
Paris
May 14, 2002
![Page 2: Technical Updates on UTEVA, TEVA and TRU Resins Anil Thakkar & Michael Fern Eichrom Technologies, Inc. Paris May 14, 2002.](https://reader035.fdocuments.in/reader035/viewer/2022062313/56649d0a5503460f949dc4c6/html5/thumbnails/2.jpg)
Topics
• UTEVA Resin: – Decontamination of Po-210 – U-232 yields
• TEVA Resin: – Decontamination of U-nat/Th in Tc-99 region
• TRU Resin: – Am recoveries
![Page 3: Technical Updates on UTEVA, TEVA and TRU Resins Anil Thakkar & Michael Fern Eichrom Technologies, Inc. Paris May 14, 2002.](https://reader035.fdocuments.in/reader035/viewer/2022062313/56649d0a5503460f949dc4c6/html5/thumbnails/3.jpg)
U-232 Yields
• Unrealistic high U-232 yields reported with UTEVA resin in samples with high in Pb-210
![Page 4: Technical Updates on UTEVA, TEVA and TRU Resins Anil Thakkar & Michael Fern Eichrom Technologies, Inc. Paris May 14, 2002.](https://reader035.fdocuments.in/reader035/viewer/2022062313/56649d0a5503460f949dc4c6/html5/thumbnails/4.jpg)
Current Procedure
1) Load sample on UTEVA resin with 10 ml of 3M HNO3/1M Al(NO3)3. with 2 mL of 0.6M Ferrous sulfamate and 200 mg of ascorbic acid.
2) Rinse sample beaker with 5 mL of 3M HNO3
3) Rinse column with 5 mL of 3M HNO3
4) Rinse column with 5 mL of 9M HCl
5) Rinse column with 20 mL of 5M HCl/0.05M Oxalic
6) Elute U with 15 mL of 0.01M HCl
![Page 5: Technical Updates on UTEVA, TEVA and TRU Resins Anil Thakkar & Michael Fern Eichrom Technologies, Inc. Paris May 14, 2002.](https://reader035.fdocuments.in/reader035/viewer/2022062313/56649d0a5503460f949dc4c6/html5/thumbnails/5.jpg)
Effect of Ferrous210Pb/210Po spike (1100 pCi)
Method Activity in URegion (dpm)
Ferrous 230
No ferrous 3.5
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Effect of Additional 3M HNO3 Rinse 210Pb/210Po spike
Activity in Uranium Region (dpm)Additional Rinse
(mL)92 pCi spike
no ferrous1080 pCi spike
ferrous
0 3.0 230
10 1.6 --
20 0.23 --
30 -- 28
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Effect of Uranium Strip Solution no ferrous added
210Pb/210Po spike (1100 pCi)
Activity in Uranium Region (dpm)
Uranium StripSolution
No ferrous ferrous
0.01M HCl 3.5 230
0.1M HCl 1.3 --
1M HCl 0.16 1.84
![Page 9: Technical Updates on UTEVA, TEVA and TRU Resins Anil Thakkar & Michael Fern Eichrom Technologies, Inc. Paris May 14, 2002.](https://reader035.fdocuments.in/reader035/viewer/2022062313/56649d0a5503460f949dc4c6/html5/thumbnails/9.jpg)
Additional Rinse/1M HCl Strip Combo
Method Activity in Uranium Region(dpm)
Original procedure 230
30 mL HNO3 Rinse only 28
1M HCl Strip only 1.84
30mL rinse + 1M Strip <background
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Revised Procedure
1) Load sample on UTEVA with 10 ml of 3M HNO3/1M Al(N03)3 with 2 mL of 0.6M Ferrous sulfamate and 200 mg of ascorbic acid
2) Rinse sample beaker with 5 mL of 3M HNO3
3) Rinse column with 5 mL of 3M HNO3
4) Rinse column with 10 mL of 3M HNO3 (3x)
5) Rinse column with 5 mL of 9M HCl
6) Rinse column with 20 mL of 5M HCl/0.05M Oxalic
7) Elute U with 15 mL of 1M HCl
![Page 11: Technical Updates on UTEVA, TEVA and TRU Resins Anil Thakkar & Michael Fern Eichrom Technologies, Inc. Paris May 14, 2002.](https://reader035.fdocuments.in/reader035/viewer/2022062313/56649d0a5503460f949dc4c6/html5/thumbnails/11.jpg)
Summary
A good decontamination of Po-210 in U-232 region can be
achieved by additional 3M HNO3 rinse on UTEVA and
eluting uranium selectively with 1M HCl
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TEVA Column: Tc-99 Issues
• Problem reported by Darrin Mann (BWXT, Oak Ridge, Tn) with bias high Tc-99 recoveries in samples with natural uranium.
• Th-234 interference was detected in Tc-99 region.
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BWXT’s Tc-99 Procedure
• Solid samples are digested and dissolved finally in 20 ml of 0.1M HNO3
• Load sample on TEVA column
• Rinse column with 25 ml of 0.1M HNO3
• Extrude resin from the column in a LSC vial.
• Add cocktail and count on LSC.
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BWXT’s Procedure tested at Eichrom
• Spiked 20 ml of 0.01M HNO3 with ~2000 dpm of U-234/238
• Load on TEVA Resin column
• Rinse with 25 ml of 0.1M HNO3
• Extrude resin in LSC vial
• Added 15 ml of cocktail and count
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Possible Solutions for Decontamination
• Use of fluoride to complex the residual Th-234 on the column
• Two fluoride solutions tested:
– Hydrofluoric acid – Sodium fluoride
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Decontamination of Th-234
• Spiked 20 ml of 0.01HNO3 with ~2000 dpm of U-234/238
• Load on TEVA Resin column
• Rinse with 5 ml of 0.1M HNO3
• Rinse with 25 ml of 0.5M HF/0.02M HNO3 OR with 25 ml of 1M NaF/0.02 HNO3
• Rinse with 5 ml of 0.1M HNO3
• Extrude resin in LSC vial
• Added 15 ml of cocktail and count
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BWXT’s ProcedureTest ResultsRinse volume used=25 mL
TEVA Lot # 0.1M HNO3
(CPM)0.5M HF
/0.02M HNO3
(CPM)
1M NaF/0.02M HNO3
(CPM)
TEA06309 72 14.84 Not tested
TE0K 18.9 13.1 15.36
TEVA Cl-
form24.5 15.36 15.0
Blank 14.7 + 0.9 14.7 + 0.9 14.7 + 0.9
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Conclusion
• Decontamination of Th-234 in Tc-99 region can be accomplished with additional fluoride rinse on the TEVA Resin columns
• Fluoride in the form of 1M NaF or 0.5M HF solutions could be used to remove the residual amounts of Th-234
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TRU Resin: History
• Historical problems with Am recoveries from TRU Resin (HCl strip.)
• Suspected Extractant Leaching handled with wet ashing of HCl Strip Solution
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TRU Resin Cartridges
1) TRU Resin
2) TRU Resin with a ‘post’ Prefilter layer
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Am-243 Spike Test
1) Spike 10 ml of 3M HNO3 with 6.52 dpm of Am-243
2) Load solution on TRU cartridges (assisted with VBS, flow rate 1ml/min)
3) Rinse with 10 ml of 3M HNO3
4) Rinse with 5ml of 0.5M HNO3
5) Strip Am with 9M + 4M HCl
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Cerium Fluoride Precipitation
Four different preparation prior to CeF3 ppt.
– 1) Digested with Aqua-regia
– 2) Undigested
– 3) Changed molarity (~0.5 M HCl)
– 4) Digested with 10% H2SO4
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Am-243 recoveries (n=4)
Resin Type Am Strip Solution
Digested with Aqua-
regia
No digestion Changed molarity
Digested with H2SO4
TRU 9M HCl + 4M HCl
89 % + 3% 48 % + 3% 97 % + 7% 84 % + 6%
TRU with prefilter layer
9M HCl + 4M HCl
89 % + 5% 62 % + 5% 97 % + 3% 82 % + 23%
![Page 24: Technical Updates on UTEVA, TEVA and TRU Resins Anil Thakkar & Michael Fern Eichrom Technologies, Inc. Paris May 14, 2002.](https://reader035.fdocuments.in/reader035/viewer/2022062313/56649d0a5503460f949dc4c6/html5/thumbnails/24.jpg)
RETEST: Am-243 recoveries (n=4)
Resin Type Am StripSolution
Changedmolarity-First Run
Changedmolarity-RERUN
TRU 9M HCl +4M HCl
97 % + 7% 93 % + 10%
TRU withprefilter layer
9M HCl +4M HCl
97 % + 3% 95 % + 4%
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ACW03 tested for Am
• 0.5 L of Eichrom tap water spiked with Am-243
• Precipitated Am with calcium phosphate
• Scavenge ppt. and dissolve in the load solution
• Followed ACW03 procedure using UTEVA/TRU cartridges
• Collect Am fraction
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ACW03…continued
6) Evaporate Am fraction to dryness
7) Add 0.5 ml of conc. HCl and dilute to 15 ml of DI water
8) Perform CeF3 ppt.
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Tap Water: Am-243 recoveries(n=5)
Resin Type Am StripSolution
Changedmolarity
UTEVA / TRU 9M HCl +4M HCl
89 % + 10%
UTEVA / TRU withprefilter layer
9M HCl +4M HCl
89 % + 11%
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Conclusion
• Am recoveries improved by changing the concentration on HCl prior to CeF3
• TRU resin cartridge performed well once the HCl concentration was changed