URANIUM IN CORAL SOIL DOE/ERSP PROCEDURENO.12 APPROVED: 1. DATE DRAFTED: 1 February 1978 4 March 1978 by John D. Stewart (ERSP Manager) Ash a 2-5 gram sample at 700°C for 10-16 hrs. Dissolve the residue in 30 ml of 8N HNOg3 and 2-3 ml of 25% NaNOo. Use 232 as the internal tracer. Transfer the sample to a 125 ml separatory funnel and add 40 ml of 30% Aliquat-336 in xylene. Shake for 5 minutes and allow phases to separate for 10-15 minutes. Drain and discard the aqueous phase. Wash the organic phase with 30 ml of 8N HNOs3. Shake for 2 minutes and allow phases to separate for 5 minutes. Drain and discard aqueous phase. Back extract the uranium from the organic phase with 50 ml of (400 ml deionized water + 16 grams oxalic acid + 80 ml HCi04) solution. Shake for 5 minutes; allow phases to separate for 10-15 minutes. Drain the aqueous phase into a 150 ml beaker. Discard organic phase. Add 1 ml of 5% NaHSOy,to the beaker containing the uranium and evaporate to near dryness. Dissolve sample with 75 ml of 9M HCl. Add 1 ml of cone HNOgandstir. q. Prepare anion exchange columnasfollows: a. To a glass column with 8-inch stem, 5/8-inch inner diameter, add a piece of glass wool to plug the stem opening. b. Make a slurry of anion resin (AG1X8 or AG1X2) in a beaker with deionized water and load on column to a height of approximately 8 em. e. Pretreat the column with 50 ml of 9M HCL Pass sample through the column. Rinse beaker with 20 ml 9M HCl and add to column. Repeat rinse one more time. Elute the uranium into 150 mi beaker with 50 ml of 1M HCi followed by a warm deionized water rinse. 10. Evaporate the solution to near dryness. 11. Electrodeposit as follows: a. Dissolve sample with 10 ml of uranium electrolyte (18 ml HNO3 + 16 ml NH4OH + 900 ml deionized water adjusted to pH 1.5). b. Agitate sample in ultrasonic cleaner. c. Transfer to a marked plating cell using the uranium electrolyte to complete the transfer. d. Electrodeposit at 300 ma for 2 hours. A-12-1