The reliabilities of two methods for measuring free acid in plutonium solutions were determined by applying each to the analysis of pluton¬ium, thorium, and cerium solutions having known free acid concentra¬tion. In the iodate method, the hydrolyzable ion was precipitated with iodate and separated by filtration, and the free acid in the filtrate was titrated with standard base. In the citrate method, the hydrolyzable ion was complexed with citrate during the titration of the free acid with standard base. Between 99 and 100% of the free acid in plutonium(IV) solutions was measured using the iodate method, and high results, 106 to 109%, were obtained using the citrate method. Neither was reliable for determining free acid in plutonium (III) solutions;the iodate method gave low results (94 to 96%), and the citrate method gave high results (108 to 109%).
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