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The determination method of free acid in spent U-Al nuclear fuel solutions by Gran plot titration was described. Effect of U(VI) and Al(III) on the alkalimetric titration of nitric acid was investigated in oxalate complexing media as well as in noncomplexing media. Positive biases were observed in b...

The determination method of free acid in spent U-Al nuclear fuel solutions by Gran plot titration was described. Effect of U(VI) and Al(III) on the alkalimetric titration of nitric acid was investigated in oxalate complexing media as well as in noncomplexing media. Positive biases were observed in both titration media when the end-point was estimated by the Gran plot method. It was found that the cause of the bias was U(VI) in the oxalate complexing media, but Al(III) in the noncomplexing media. The relative error was less than 1% in the titration of 0.1 M $HNO_3$ at a U(VI) : Al(III) : $H^+$ mole ratio of up to 2:12:1 as long as the pH of the oxalate titration media was sustained to be below 5.0 at the beginning of titration. The method was successfully applied to the determination of nitric acid in a solution of HANARO reactor fuel with U:Al mole ratio of 1:6.

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