A second-derivative spectrophotometric method has been developed for the simultaneous determination of uranium and thorium using 4-(2'-thiazolylazo)resacetophenone oxime as the spectrophotometric reagent. The method allows the determination of uranium and thorium in the range 0-10.0 ppm. The relative error is less than 4%. Common anions and cations do not interfere in the determination even when present in large amounts. However, for transition metal ions, viz., Cu, Ni, Pd and Pt, the tolerance limit is less than 100 ppm.

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