AM IN CORALSOIL DATE DRAFTED: 30 January 1978 DOE/ERSP PROCEDURE NO.11 APPROVED: L 11 February 1978 by Don R. Martin (ERSP Manager) Introduction Americium-243 tracer must be added to the sample during the initial dissolution, prior to the plutonium extraction. If no plutonium analysis is to be performed, the sample may be diluted immediately following the initial dissolution. Reagents NH,0H 1.5M HNO3g Fe Clg solution 2M HNO3 HCl 6M HNOg 0.5M HNO3 8M HNO3 50Wx8 Dowex Resin (50-100 mesh) Il. Procedure 1. 2. 3. Dilute the 8M HNOg from the plutonium extraction to 100 ml. Aliquot 20 ml into a 40 ml centrifuge tube. Add approximately 10 mg Fe carrier and stir. Precipitate Fe(OH)3 with NH4OH. Digest the sample in hot bath for 5 minutes. Centrifuge sample and discard the supernate. Dissolve the sample in 5 ml HNO3. Digest in a hot bath for 5 minutes. Dilute the sample to 20 ml with deionized water. Add NH4OH to precipitate Fe(OH)3. Centrifuge sample and discard supernate. 4. Dissolve the sample with 15 ml concentrated HCl and 1 drop concentrated HNOg3 and pass the sample through an ion exchange column pretreated with concentrated HCl. (The resin is BioRad 1x2 50-100 mesh, resin bed is 10 em x 12 mm.) Collect the load solution and one 10 ml wash of concentrated HCl. 5. 6. Evaporate the sample to dryness. Add 5 ml HNOs, and 5 ml HCl. Evaporate the sample to incipient dryness. Dissolve the sample with 25 ml of 0.5M HNOs. Pass the sample through a cation exchange resin column (Note 1). Wash the column with 25 ml 0.5M HNOx3. 2M HNOg. 7. Wash the column with 100 ml 1.5M HNO3. Wash the column with 20 ml of _Elute the americium into a 250 ml beaker with 100 ml 6M HNO3. Evaporate the sample to dryness. : 8. Transfer the sample to a 40 mi centrifuge tube with 5 ml HNOg3 and deionized water. Add approximately 10 mg Fe carrier. Precipitate Fe(OH)3 by adding NH4OH. Centrifuge the sample and discard the supernate. 9. Repeat step 4. 10. Add 5 ml conc HNOs, evaporate to dryness and prepare the sample for electrodeposition. A-11-1