rapid actinide analysis for large soil samples-update
DESCRIPTION
Rapid Actinide Analysis for Large Soil Samples-Update. Sherrod L. Maxwell, III Westinghouse Savannah River Company. SRS Soil Method. Total Dissolution High recoveries Faster Sample preparation Good alpha resolution Effective removal of interferences such as Th isotopes and Po-210. - PowerPoint PPT PresentationTRANSCRIPT
![Page 1: Rapid Actinide Analysis for Large Soil Samples-Update](https://reader035.vdocuments.net/reader035/viewer/2022070418/56815822550346895dc58928/html5/thumbnails/1.jpg)
Rapid Actinide Analysis for Large Soil Samples-Update
Sherrod L. Maxwell, III
Westinghouse Savannah River Company
![Page 2: Rapid Actinide Analysis for Large Soil Samples-Update](https://reader035.vdocuments.net/reader035/viewer/2022070418/56815822550346895dc58928/html5/thumbnails/2.jpg)
SRS Soil Method
• Total Dissolution
• High recoveries
• Faster Sample preparation
• Good alpha resolution
• Effective removal of interferences such as Th isotopes and Po-210
![Page 3: Rapid Actinide Analysis for Large Soil Samples-Update](https://reader035.vdocuments.net/reader035/viewer/2022070418/56815822550346895dc58928/html5/thumbnails/3.jpg)
Update-Improvements
• Enhancements to improve precipitation steps
• Better Am recovery for difficult samples– DGA Resin added to column method
![Page 4: Rapid Actinide Analysis for Large Soil Samples-Update](https://reader035.vdocuments.net/reader035/viewer/2022070418/56815822550346895dc58928/html5/thumbnails/4.jpg)
Transfer to crucible after silicon removal
![Page 5: Rapid Actinide Analysis for Large Soil Samples-Update](https://reader035.vdocuments.net/reader035/viewer/2022070418/56815822550346895dc58928/html5/thumbnails/5.jpg)
10 grams sodium peroxide + 5 grams sodium hydroxide
700C for 20 minutes
![Page 6: Rapid Actinide Analysis for Large Soil Samples-Update](https://reader035.vdocuments.net/reader035/viewer/2022070418/56815822550346895dc58928/html5/thumbnails/6.jpg)
Just add water after cooling briefly
![Page 7: Rapid Actinide Analysis for Large Soil Samples-Update](https://reader035.vdocuments.net/reader035/viewer/2022070418/56815822550346895dc58928/html5/thumbnails/7.jpg)
Dilute to 1 liter with water with iron carrier (increased to 150-250 mg), TiCl3, and barium (1.5 mL of 10%) present, add 5-10 mg Ce
![Page 8: Rapid Actinide Analysis for Large Soil Samples-Update](https://reader035.vdocuments.net/reader035/viewer/2022070418/56815822550346895dc58928/html5/thumbnails/8.jpg)
After centrifuging, acidify and add TiCl3, Ce (2mg) and HF.
![Page 9: Rapid Actinide Analysis for Large Soil Samples-Update](https://reader035.vdocuments.net/reader035/viewer/2022070418/56815822550346895dc58928/html5/thumbnails/9.jpg)
Place on ice, then centrifuge
![Page 10: Rapid Actinide Analysis for Large Soil Samples-Update](https://reader035.vdocuments.net/reader035/viewer/2022070418/56815822550346895dc58928/html5/thumbnails/10.jpg)
Rinse with 0.25M HCL-3.8M HF-0.04M rongalite
![Page 11: Rapid Actinide Analysis for Large Soil Samples-Update](https://reader035.vdocuments.net/reader035/viewer/2022070418/56815822550346895dc58928/html5/thumbnails/11.jpg)
Redissolve in acid, boric acid and aluminum nitrate
![Page 12: Rapid Actinide Analysis for Large Soil Samples-Update](https://reader035.vdocuments.net/reader035/viewer/2022070418/56815822550346895dc58928/html5/thumbnails/12.jpg)
Actinides in Soil
RinseBeaker rinse: 3mL 6MHN03
Separate cartridges:TEVA: 5 mL 3MHN03 Collect/acidify - with 2 mL16M HN03 then to TRUTEVA:10 mL 5M HNO3 Discard
10 mL 3M HN03 Discard
Th Elution20mL 9MHCI
Pu (and/or Np) Elution20mL
0.10MHC1 - 0.05MHF - 0.03M TiCl3
1) Redissolve in 5 mL warm 3M HN03 - 0.25M boric acid, add 6mL 7M HNO3 and 7.5 mL 2M Al(N03 ) 3
2) Add 0.5 mL 1.5M Sulfamic Acid + 1.25 mL 1.5M Ascorbic Acid3) Add 1 mL 3.5 M Sodium Nitrite
2 mL TEVA Resin(50-100 um)
2 mL TRU-Resin (50-100 um)
Alpha spectrometry
Cerium fluoride
Add 0.5 mL 30 wt% H2O2
2 mL DGA-Resin (50-100 um)
![Page 13: Rapid Actinide Analysis for Large Soil Samples-Update](https://reader035.vdocuments.net/reader035/viewer/2022070418/56815822550346895dc58928/html5/thumbnails/13.jpg)
Actinides in Soil with DGA
Remove TRU and DGA cartridge:
1) Rinse TRU+ DGA with 3 mL of 3M HNO3 and discard rinse.
2) Elute any U from DGA only with 6 mL of 0.25M HNO3 (then add 5 mL con. HNO3 to adjust acid)
3) Elute Am from DGA only with 10 mL 0.1M HCl. Add 4 mL of con. HCl to soln. To adjust acid to 3.5 M HCl.
4) Add DGA strip solution (con HCL added) to TRU to strip Am from TRU, recombine Am. Rinse TRU with 3M HCl.
![Page 14: Rapid Actinide Analysis for Large Soil Samples-Update](https://reader035.vdocuments.net/reader035/viewer/2022070418/56815822550346895dc58928/html5/thumbnails/14.jpg)
Actinides in Soil with DGA, Cont.
5) Add 3M HNO3 rinse (then adj. ~7M HNO3) from TEVA to load to TRU
6) Add U fraction from DGA adjusted to ~ 7M HNO3 to add any U from DGA to TRU and remove any Po-210.
7) Add 18 mL 4M HCl-0.2M HF to TRU to remove Th
8) Elute U with 15mL 0.1M ammonium bioxalate
![Page 15: Rapid Actinide Analysis for Large Soil Samples-Update](https://reader035.vdocuments.net/reader035/viewer/2022070418/56815822550346895dc58928/html5/thumbnails/15.jpg)
Load with TEVA+TRU+DGA
Split Apart TEVA and TRU/DGA
![Page 16: Rapid Actinide Analysis for Large Soil Samples-Update](https://reader035.vdocuments.net/reader035/viewer/2022070418/56815822550346895dc58928/html5/thumbnails/16.jpg)
Rinse, then strip Pu from TEVA
Strip Am/Cm fromDGA/add acid/thenpass thru TRU
![Page 17: Rapid Actinide Analysis for Large Soil Samples-Update](https://reader035.vdocuments.net/reader035/viewer/2022070418/56815822550346895dc58928/html5/thumbnails/17.jpg)
Am/RE Removal on TEVA
Rinse
Beaker rinse: 3mL 4M NH4SCN, warm
10 mL 1.5 M NH4SCN to column
Am Elution25 mL 1M HCl
(warm and rinse original beaker)
1) Evaporate 4M HCl with 5mL con.HNO3, 50 uL of 1.8M H2SO4, then ash with nitric acid and hydrogen peroxide
2) Redissolve in 5 mL of 4M NH4SCN, warm gently.
2mL TEVA Resin(50-100 um)
Alpha spectrometry
Cerium fluoride
![Page 18: Rapid Actinide Analysis for Large Soil Samples-Update](https://reader035.vdocuments.net/reader035/viewer/2022070418/56815822550346895dc58928/html5/thumbnails/18.jpg)
Final Am Clean-up on TEVA
![Page 19: Rapid Actinide Analysis for Large Soil Samples-Update](https://reader035.vdocuments.net/reader035/viewer/2022070418/56815822550346895dc58928/html5/thumbnails/19.jpg)
10 g sample
![Page 20: Rapid Actinide Analysis for Large Soil Samples-Update](https://reader035.vdocuments.net/reader035/viewer/2022070418/56815822550346895dc58928/html5/thumbnails/20.jpg)
5 g sample-Resolve Filters
![Page 21: Rapid Actinide Analysis for Large Soil Samples-Update](https://reader035.vdocuments.net/reader035/viewer/2022070418/56815822550346895dc58928/html5/thumbnails/21.jpg)
5 g sample-Resolve Filters
![Page 22: Rapid Actinide Analysis for Large Soil Samples-Update](https://reader035.vdocuments.net/reader035/viewer/2022070418/56815822550346895dc58928/html5/thumbnails/22.jpg)
MAPEP samplewith DGA
![Page 23: Rapid Actinide Analysis for Large Soil Samples-Update](https://reader035.vdocuments.net/reader035/viewer/2022070418/56815822550346895dc58928/html5/thumbnails/23.jpg)
MAPEP samplewith DGA
![Page 24: Rapid Actinide Analysis for Large Soil Samples-Update](https://reader035.vdocuments.net/reader035/viewer/2022070418/56815822550346895dc58928/html5/thumbnails/24.jpg)
MAPEP samplewith DGA
![Page 25: Rapid Actinide Analysis for Large Soil Samples-Update](https://reader035.vdocuments.net/reader035/viewer/2022070418/56815822550346895dc58928/html5/thumbnails/25.jpg)
Summary
• Enhanced precipitation steps– Cerium added during iron hydroxide ppt.
• Increased for sandy samples
– Increased barium during iron hydroxide ppt.– lower HF/increased rongalite in final rinse of
cerium fluoride ppt.
• Improved Am recoveries– DGA resin