THE RADIOCHEMISTRY OF PLUTONIUM - Sciencemadness.org

Notes
11. Prepare an eluting solution containing 20 ml HCl and 75 mg NH41,
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a.
HN03 . Rinse the tube tith several 1-ml portions of this solution.
Transfer these washes to the column. Wash the column with the
remaining solution in 2-ml portions. Wash with 15 ml HC1 in Z-ml
portions. Discard the effluents and washes.
Elute the Pu from the column into a 50-ml beaker with 2-ml portions
of this solution, allowing the first 2 -ml portion to pass through. Add
the second 2-ml portion and plug the top of the column with a piece of
pressure -senfiitive tape for 5 min. Remove the tape and continue to
elute in 2-ml portions. Pass through 6 ml of HC1 in 2-ml portions.
Add 2 mg of La and evaporate the solution to approximately 5 ml.
Transfer to a 50-ml lusteroid tube and dflute to a volume of 10 ml.
Add 20 mg NaHS03 a little at a time.
Add 10 drops HF with stirring, and Wow to stand for a few minutes.
Cool in an ice bath, centrifuge, and wash the LaF3 with 2 ml 1~ HC1
Xl~HF. Discard the supernate and wash.
Repeat Steps 7 through 11.
Evaporate the solution in the 50-ml beaker to approximately 5 rnls with
addition of HNO to drive off all iodine. Transfer the solution to a 40
3
ml centrifuge tube.
Add 5 mg Fe+++ and precipitate Fe(OH)3 by addition of NH40H .
Digest in a hot water bath for a few minutes. Centrifuge, and wash
tb~ precipitate with 5 ml water containing 1 drop NH40H. Discard the
supernate.
Dissolve the Fe(OH)3 in 5 ml 6 ~ HN03 . Add 4 drops saturated NaBr03
solution. Warm on a hot water bath for a few minutes. Saturate the
solution with NTH4N03 crystals, add 5 ml hexone (methyl isobutyl
ketone) and stir with a mechanical stirrer for 3 min. Centrifuge to
separate the phases, and withdraw the hexone (upper) layer with a
transfer pipet. Transfer the hexone to a clean, dry 40-ml centrifuge
tube.. Repeat the extraction twice, adding 1 drop of saturated NaBr03
and more NH4N03 if necessary.
Record the time of extraction as the “ Final Separation of Pu 241 and
Am241 ,,
Wash the hexone phases by stirring with 5 ml 6 ~ HN03 . Stir for 2
rein, centrifuge, withdraw the acid (lower) phase and combine with
original aqueous phase.
Back-extract the Pu from the hexone by stirring for 3 min with 5 ml
O.1~ HN03. Centrifuge, and transfer the aqueous phase into a 50-ml
beaker. Repeat twice and combine the aqueous phases.
The solution is now ready for electroplating.
Do not continue step 3 unless there is enough time to carry the
procedure completely and rapidly through step 5.
b. Dissolve 1 granule of Na2CR207 with 1/2 ml HF in a Pt dish.
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