THE RADIOCHEMISTRY OF PLUTONIUM - Sciencemadness.org

Procedure 22. Determination of Americium in Urine in the Presence of Plutonium
D. L. Bowkowski (Ref. 53).
Outline of Method
The Pu is co-precipitated with BiP04 from acidified urine, the BiP04
is wet-ashed with HN03, and the Pu is co-precipitated with LaF3 from an HC1
solution. The LaF3 co-precipitation is repeated and the fluoride is metathesized with
KOH. Pu is extracted into di(2- ethylhexyl)phosphoric acid from a 2 ~ HN03 solution,
and the aqueous phase is mounted for counting.
This procedure is included to illustrate the extraction of Pu(IV) into acidic
phosphate extract ants. The procedure could presumably be used for a simultaneous
determination of Pu and Am in urine, by back-extraction of the Pu either into strong
acid or a reducing solution.
Reagents
Bromthymol blue indicator solution – Dissolve one g of reagent grade
indicator in 500 ml of distilled water made alkaline with one pellet of sodium hydroxide.
Bismuth nitrate solution – Dissolve 231.2 g of bismuth nitrate [ Bi(N03 )3. 5H20-AR]
in 660 ml of concentrated HNO and dilute
3
to one liter with distilled water.
solution contains O. 1 g of Bi per ml.
4 ~ HC1 – Add 344 ml of cone. HC1 to approximately 500 ml of distilled water in
a volumetric flask and make up to 1 liter with distilled water.
6 ~ HCl – Dilute 510 ml of cone. HC1 to 1 liter in a volumetric flask.
8 ~ HC1 – Dilute 688 ml of cone. HC1 to 1 liter in a volmnetric flask.
Lanthanum nitrate solution – La(N03 )3, as received from the Lindsey Chemical
Company, West Chicago, Illinois, is freed from actinum a-emitting impurities on a
Dowex 50X12 cation exchange resin column by the method of Farabee. * The lanthanum
nitrate stock solution obtained is used to prepare working solutions containing 25 mg of
La++/ ml. Only solutions containing 0.05 d/rein or less of a activity per mg of La+++
are used.
2 M Hydroxylamine hydrochloride – Dissolve 139.0 g of C. P. grade hydroxylamine
—
hydrochloride and dilute to one liter. Store in brown bottle.
2 ~ Sodium nitrite solution – Dissolve 13.8 g of sodium nitrite (NaN02-AR) in
distilled water in a 100-ml volumetric flask and make to volume with distilled water.
Prepare fresh before use.
O. 1 M D2EHPA – Add 32.3 g of di(2-ethylhexyl) phosphoric acid (Union Carbide
—
Chemical Company) to chloroform-AR in a 1-liter volumetric flask and make to volume
with chloroform.
8 ~ KOH – Dissolve 65.3 g of potassium hydroxide (KOH 86% -AR) in distilled
water and dilute to 1 liter.
All other chemicals are either of reagent or C. P. quality.
* L. B. Farabee, 5th Ann. Meeting-Bioassay and Analyt. Chem. Grp. , Oct. 1-2,
1,959 (USAEC Report TID-7591 Nov. 1960 p. 78).
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