Procedure 2. Separation and determination of Pu by TTA extraction

The sample is pre-treated if necessary, with either H Og or by precipitating LaF3 and dissolving in A1(N03)3-HN03. The pre-treatment destroys any polymer vidiich may be present and assures the proper valence state (IV) for the TTA extraction. Pu(IV) is extracted from 2 M HNO3 and stripped into 10 M HNO3, evaporated onto a plate, and counted. Yield is quantitative. 

Hydroxylamine hydrochloride, 1 M, is prepared by dissolving 69.5 grams of C.P. grade and diluting it to 1 liter. 

2-Thenoyltrifluoroacetone-xylene 0.5M. is prepared by dissolving 111 grams of the ketone and diluting it to 1 liter with C. P. xylene. (2-Thenoyltrifl.uoro acetone may be obtained from Graham, Crowley, and Associates, Inc., 5465 West Division St., Chicago 51, HI.) 

Nitric acid method. A suitable aliquot of the sample solution is pipetted into a 100-ml volumetric flask containing 13 ml of concentrated nitric acid. The solution is heated carefiilly to a low boil on a hot plate and the temperature is held just under boiling for 5 min. The solution is then made to a known volume with distilled water. The nitric acid concentration of this solution should be approximately 2M. 

---