Modified titrimetric determination of plutonium using photometric end-point detection

Abstract

A method used at LASL for the accurate and precise assay of plutonium metal was modified for the measurement of plutonium in plutonium oxides, nitrate solutions, and in other samples containing large quantities of plutonium in oxidized states higher than +3. In this modified method, the plutonium oxide or other sample is dissolved using the sealed-reflux dissolution method or other appropriate methods. Weighed aliquots, containing approximately 100 mg of plutonium, of the dissolved sample or plutonium nitrate solution are fumed to dryness with an HC1O/sub 4/-H/sub 2/SO/sub 4/ mixture. The dried residue is dissolved in dilute H/sub 2/SO/sub 4/, and the plutonium is reduced to plutonium (III) with zinc metal. The excess zinc metal is dissolved with HCl, and the solution is passed through a lead reductor column to ensure complete reduction of the plutonium to plutonium (III). The solution, with added ferroin indicator, is then titrated immediately with standardized ceric solution to a photometric end point. For the analysis of plutonium metal solutions, plutonium oxides, and nitrate solutions, the relative standard deviation are 0.06, 0.08, and 0.14%, respectively. Of the elements most likely to be found with the plutonium, only iron, neptunium, and uranium interfere. Small amounts of uraniummore » and iron, which titrate quantitatively in the method, are determined by separate analytical methods, and suitable corrections are applied to the plutonium value. 4 tables, 4 figures.« less