11. Electrodeposit sample for 4 hours at 180 ma. 12. After 4 hours and with eurrent still on, add two drops of phenolphthalein indicator and make basie with 1% NH4OH. Empty cell and wash twice with 10 ml of deionized water. 13. Remove dise and rinse with water, followed by an alcohol rinse. Allow to air dry. 14, Flame dise at low heat until disc turns a gold color; cool. 15. Count in alpha spectrometer for 400 minutes. NOTE1: The resin bed is Dowex 50Wx8 50-100 mesh 12mmx18em. The column is pretreated by pouring through 20 ml 8M HNOs, followed by 25 ml deionized water. completes the pretreatment. 25 ml of 0.5M HNO3 CORAL SAMPLE ANALYSIS FOR AM DATE DRAFTED: 19 January 1979 DOE/ERSP PROCEDURENO.11.1 APPROVED: L 29 January 1979 by Ernie Campbell (ERSP Manager) Introduction This procedure supersedes DOE/ERSP Procedure No. 11. This procedure guarantees the complete separation and purification of the americium isotopes from other interfering radionuclides. 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. IL. Procedure 1. 2. Adjust the volume of the 8M HNOg3fraction from the plutonium extraction step to 100 ml with 8M HNOg. Transfer a 20 ml aliquot into a 40 ml centrifuge tube. Add approximately 10 mg of Fe carrier and stir. Adjust the pH to 9-11 with cone NH4OH. Place sample in a hot water bath and digest for 5 minutes. Cool sample, centrifuge and discard the supernatant. 3. Dissolve the precipitate in 5 ml of cone HNO3. Digest in a hot water bath for 5 minutes. Add 20 ml of deionized water. Adjust the pH to 9-11 with 12M NaOH and allow to digest in hot water bath for another 5 minutes. Cool sample, centrifuge and discard supernatant. 4. Wash the precipitate with 10 ml of deionized water, centrifuge and discard the supernatant. 5. Dissolve the precipitate in 5 ml of cone HNOg and three drops of cone HCl. Place in a hot water bath and digest for 5 minutes. Add 20 ml of deionized water. Adjust pH to 9-11 with cone NH4OH and allow to digest for another 5 minutes. Cool sample, centrifuge and discard the supernatant. 6. Dissolve the precipitate in 15 ml cone HCl and 1 drop conc HNOg, 7. Prepare an anion exchange column with a 12mm x 10cm bed of BioRad AG1X2, 50-100 mesh resin. Wash the column with 50 ml cone HCl. 8. Pass sample through resin column and collect the eluate in a 250 ml beaker. Wash the column with two 10 ml portions of conc HCl. Collect the HCl washes in the same beaker. 9. Evaporate the sample to near dryness. Add 5 ml cone HNOg and 5 ml cone HCl. Evaporate to near dryness. Dissolve sample in 25 ml of 0.5M HNQOg3. A-11-2