Rapid Actinide Analysis for Large Soil Samples-Update

1. Rapid Actinide Analysis for Large Soil Samples-Update Sherrod L. Maxwell, III Westinghouse Savannah River Company

2. SRS Soil Method • Total Dissolution • High recoveries • Faster Sample preparation • Good alpha resolution • Effective removal of interferences such as Th isotopes and Po-210

3. Update-Improvements • Enhancements to improve precipitation steps • Better Am recovery for difficult samples • DGA Resin added to column method

4. Transfer to crucible after silicon removal

5. 10 grams sodium peroxide + 5 grams sodium hydroxide 700C for 20 minutes

6. Just add water after cooling briefly

7. 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

8. After centrifuging, acidify and add TiCl3, Ce (2mg) and HF.

9. Place on ice, then centrifuge

10. Rinse with 0.25M HCL-3.8M HF-0.04M rongalite

11. Redissolve in acid, boric acid and aluminum nitrate

12. Actinides in Soil 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 Acid 3) Add 1 mL 3.5 M Sodium Nitrite Rinse Beaker rinse: 3mL 6MHN03 Separate cartridges: TEVA: 5 mL 3MHN03 Collect/acidify - with 2 mL16M HN03 then to TRU TEVA:10 mL 5M HNO3 Discard 10 mL 3M HN03 Discard Th Elution 20mL 9MHCI Pu (and/or Np) Elution 20mL 0.10MHC1 - 0.05MHF - 0.03M TiCl3 Add 0.5 mL 30 wt% H2O2 2 mL TEVA Resin (50-100 um) Cerium fluoride Alpha spectrometry 2 mL TRU-Resin (50-100 um) 2 mL DGA-Resin (50-100 um)

13. 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.

14. 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

15. Load with TEVA+TRU+DGA Split Apart TEVA and TRU/DGA

16. Rinse, then strip Pu from TEVA Strip Am/Cm from DGA/add acid/then pass thru TRU

17. Am/RE Removal on TEVA 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. Rinse Beaker rinse: 3mL 4M NH4SCN, warm 10 mL 1.5 M NH4SCN to column Am Elution 25 mL 1M HCl (warm and rinse original beaker) 2mL TEVA Resin (50-100 um) Cerium fluoride Alpha spectrometry

18. Final Am Clean-up on TEVA

19. 10 g sample

20. 5 g sample- Resolve Filters

21. 5 g sample-Resolve Filters

22. MAPEP sample with DGA

23. MAPEP sample with DGA

24. MAPEP sample with DGA

25. 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