Procedure 21. Determination of Plutonium in Urine

A 24-hr sample of urine is dried and ashed and the residue dissolved in dil. HCl and adjusted to a pH of 1. The Pu is reduced to the trivalent state with hydroxylamine hydrochloride solution and co-precipitated on iron cupferride. This is extracted with chloroform, the chloroform is distilled off, and the cupferrides residue is wet oxidized. The iron carrying the Pu is finally mo inted with cone. HCl, dried, precipitated with ammonium hydroxide, dried again, and flamed off to FejOg. This 

Ferric chloride solution. 145 mg of FeClg/liter (i. e. 50 mg Fe/liter). Hydroxylamine hydrochloride solution. 50 g of NHgOH- HCl/liter. Cupferron. 5% aqueous solution, renewed weekly. 

Evaporate a 24-hr sample of urine overnight in a 2-liter porcelain basin under infrared lamps. 

When dry, scrape out and quantitatively transfer the residue to a 200-ml silica dish with washings of 4 N HCl, and re-dry it under infrared lamps. 

Place the sample in a muffle furnace at 500°C, and hasten oxidation by periodic additions of 3-ml lots of cone. HNOg to the dish when it is cool. 

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