The effect of ion-exchange purification on the determination of plutonium at the New Brunswick Laboratory
Mitchell, W.G.; Spaletto, M.I.; Lewis, K.; Soriano, M.D.; Smith, M.W.
USDOE New Brunswick Lab., Argonne, IL (USA)1990
USDOE New Brunswick Lab., Argonne, IL (USA)1990
AbstractAbstract
[en] The method of plutonium (Pu) determination at the Brunswick Laboratory (NBL) consists of a combination of ion-exchange purification followed by controlled-potential coulometric analysis (IE/CPC). The present report's purpose is to quantify any detectable Pu loss occurring in the ion-exchange (IE) purification step which would cause a negative bias in the NBL method for Pu analysis. The magnitude of any such loss would be contained within the reproducibility (0.05%) of the IE/CPC method which utilizes a state-of-the-art autocoulometer developed at NBL. When the NBL IE/CPC method is used for Pu analysis, any loss in ion-exchange purification (<0.05%) is confounded with the repeatability of the ion-exchange and the precision of the CPC analysis technique (<0.05%). Consequently, to detect a bias in the IE/CPC method due to the IE alone using the IE/CPC method itself requires that many randomized analyses on a single material be performed over time and that statistical analysis of the data be performed. The initial approach described in this report to quantify any IE loss was an independent method, Isotope Dilution Mass Spectrometry; however, the number of analyses performed was insufficient to assign a statistically significant value to the IE loss (<0.02% of 10 mg samples of Pu). The second method used for quantifying any IE loss of Pu was multiple ion exchanges of the same Pu aliquant; the small number of analyses possible per individual IE together with the column-to-column variability over multiple ion exchanges prevented statistical detection of any loss of <0.05%. 12 refs
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Jul 1990; 54 p; OSTI as DE91009061; NTIS; INIS; US Govt. Printing Office Dep
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