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Yamamoto, Masahiko; Holland, M. K.*; Cordaro, J. V.*; Kuno, Takehiko; Surugaya, Naoki
JAEA-Technology 2017-014, 63 Pages, 2017/06
JAEA-Technology-2017-014.pdf:4.38MB
In this study, the controlled-potential coulometry has been applied as a primary method for characterizing the Pu master solutions being used as alternative source material for IDMS spikes. The coulometry system compliance with ISO12183 has been used for measurement. It has been calibrated using equipment traceable to the SI units. Plutonium standard samples have been measured to confirm the accuracy. The relative standard deviation is below 0.05%. The results agree with the reference value within 
0.05%. It is found that the Pu can be precisely analyzed by the coulometry system. Then, the Pu nitrate solution, which has been purified from mixed oxide powder containing relatively high 
Pu, has been measured. The relative standard deviation is below 0.05%. The relative expanded uncertainty is less than 0.074% at the 95% confidence interval (k=2). It is indicated that coulometric assay of Pu is fit for the purpose of characterizing reference materials.
Yamamoto, Masahiko; Holland, M. K.*; Cordaro, J. V.*; Kuno, Takehiko; Surugaya, Naoki
Dai-37-Kai Kaku Busshitsu Kanri Gakkai Nihon Shibu Nenji Taikai Rombunshu (CD-ROM), 9 Pages, 2017/02
Precise and accurate determination of plutonium is necessary. The high reliability is required for standard materials used in the plutonium determination. In this study, JAEA and SRNL have collaborated on a mission to apply controlled-potential coulometry as a primary method for characterizing the plutonium master solution being used for reference materials of isotope dilution mass spectrometry. The measurement cell and electrodes were upgraded and optimized compliance with ISO12183. The instruments were calibrated traceable to the SI. The samples of plutonium standard solution were measured to confirm the accuracy of the method. The results have been in good agreement with the reference values. Therefore, the plutonium solution which were purified from MOX powder have been characterized. The total measurement uncertainty was less than 0.07%. The results indicated that coulometry assay of plutonium are fit for the purpose of characterizing reference material.