Improvement of precision spectrophotometric method with internal reference and its application to analysis of plutonium solutions

A spectrophotometric precision method with internal reference [1, 2] was applied to analysis of straight Pu solutions for certifying Pu reference materials and for studying the PuO₂ solubility in the framework of developing methods for accounting and control of nuclear materials. In the context of the activities mainly concerned with certification of reference materials, a two-channel spectrophotomer and the corresponding technique were further improved in order to decrease the error of the method. This allowed the random component of the relative error of the method to be decreased from 0.1 to 0.04% at the confidence level p = 0.95 and the number of degrees of freedom f = 25. The fixed component of the error of the method was studied in relation to impurities of U, Np and corrosion products of structural materials. Also, the extent of Pu oxidation during sample preparation was studied as influenced by the fluoride ion. The revealed lack of such influence within the limits of the study indicates that the method is suitable for analysis of Pu in mixed solutions.