PLUTONIUM IN URINE DATE DRAFTED: 30 January 1978 DOE/ERSP PROCEDURENO, 14 APPROVED: 16 February 1978 by Don R. Martin (ERSP Manager) Transfer the sample into a 2 liter graduated cylinder. Make certain the entire sample is transferred. 2. Check acidity of sample using pH paper. If the sample is not acidic (at least pH 2.) cautiously add with a swirling motion 4 ml of cone HNO3 per 100 ml of sample. N-octyl alcohol may be added if excessive foaming occurs. Mix sample well. Record the acidified volume on sample sheet. Pour 700 mi of urine into a 1000 ml graduate tall form beaker. a. If sample is < 700 ml transfer entire sample into a 1000 ml tall form beaker. Record the aliquot used on the sample sheet. Add ten drops of calcium carrier (111 g Ca (NO3)9 in 200 ml deionized water). Add 236 py internal tracer and 1 ml of 85% H3P0q . Place sample on hot plate and stir continuously. When temperature of sample is between 70 -80°C add approximately 200 ml of cone NH4OH to pH of 9-10. Allow sample to digest for 30 minutes with continuous stirring. 10. Allow sample to stand at least 16 hours, decant and discard liquid. 11, Dissolve the precipitate with 20 ml of 8N HNOg. Evaporate sample to incipient dryness, 12. Continue wet ashing sample with cone HNO3 and HQ, until a white residue is obtained (muffle may be used at low temperature to speed up ashing). 13. Dissolve sample in 30 ml of 8N HNOg; add 2-3 ml of 25% NaNOg. allow to cool. 14. Transfer to a 125 ml separatory funnel and rinse beaker with 8N HNO3. Transfer rinse to separatory funnel. a. b. Heat sample and Add 40 mi of 30% Aliquat-336 in xylene. Shake for 5 minutes and let the sample stand for 10 minutes. Phase (bottom layer). Discard the aqueous ¢. Add 30 ml of 8N HNOg and shake for 2 minutes. Let stand for 5 minutes. Discard d. Backextract the plutonium from the organic phase with 50 ml portion of HClO4 oxalic acid solution (400 ml water and 80 ml cone HClOqg to 16 grams of oxalic acid). Collect the backextract in a 100 ml beaker. Discard the organic waste. the aqueous phase. 15. Add 1 ml 5% NaHSQyq solution to sample and evaporate to dryness in the perchloric acid fume hood. 16. Dissolve the sample with 50 ml of 8N HNO3. A-14-1