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Journal Articles

Accurate and precise measurement of uranium content in uranium trioxide by gravimetry; Comparison with isotope dilution mass spectrometry and its uncertainty estimation

Yamamoto, Masahiko; Horigome, Kazushi; Kuno, Takehiko

Applied Radiation and Isotopes, 190, p.110460_1 - 110460_7, 2022/12

 Times Cited Count:0 Percentile:0.01(Chemistry, Inorganic & Nuclear)

Gravimetric measurement of U content in UO$$_{3}$$ with ignition in the air has been investigated. The ignition temperature, ignition time and aliquot sample mass are optimized as 900$$^{circ}$$C, 60 minutes, and 1 g, respectively. The method is validated by IDMS with uncertainty estimation. The obtained result by gravimetry is 0.78236$$pm$$0.00051 g/g (k=2) and agreed with IDMS value within its uncertainty. It has been found that U in UO$$_{3}$$ can be measured accurately and precisely by gravimetry.

Journal Articles

Separation technique using column chromatography for safeguards verification analysis of uranium and plutonium in highly-active liquid waste by isotope dilution mass spectrometry

Yamamoto, Masahiko; Taguchi, Shigeo; Horigome, Kazushi; Kuno, Takehiko

Proceedings of IAEA Symposium on International Safeguards; Building Future Safeguards Capabilities (Internet), 8 Pages, 2018/11

In this study, the single-column extraction chromatographic separation has been developed for analysis of U and Pu in highly active liquid waste by isotope dilution mass spectrometry (IDMS). The commercially available TEVA$$^{textregistered}$$ resin is selected as an extraction chromatography resin. The U is chromatographically separated from fission products (FP) elements by nitric acid while Pu(IV) is adsorbed on the resin. After that, Pu is eluted by reducing to Pu(III). The method has been successfully achieved the separation with yielding the enough recovery and sufficient decontamination factors for subsequent IDMS analysis. The column dose rate after the FP removal is decreased to the background. The analytical results obtained by the developed method are in a good agreement with those of the conventional method. It provides simple and rapid separation and expected that the method can be applied to join IAEA/Japan on-site analytical laboratory.

JAEA Reports

Preparation of uranium and plutonium mixed spike optimized for MOX analysis by isotope dilution mass spectrometry

Horigome, Kazushi; Taguchi, Shigeo; Yamamoto, Masahiko; Kuno, Takehiko; Surugaya, Naoki

JAEA-Technology 2017-016, 20 Pages, 2017/07


Mixed spikes of uranium and plutonium have been prepared for the determination of uranium and plutonium in dissolved MOX solution by isotope dilution mass spectrometry. Enriched uranium metal NBL CRM116 and plutonium metal NBL CRM126 were accurately weighed and then dissolved in nitric acid, respectively. Their dissolved solutions were mixed in a mass ratio of 1 to 2. The preparation values of uranium and plutonium were 1.0530 $$pm$$ 0.0008 mg/g (k=2) of uranium with a $$^{235}$$U relative mass fraction of 93.114 wt% and 2.0046 $$pm$$ 0.0019 mg/g (k=2) of plutonium with a $$^{239}$$Pu relative mass fraction of 97.934 wt%, respectively. The concentrations of uranium and plutonium in spike were confirmed by reverse isotope dilution mass spectrometry using tracer of $$^{233}$$U and $$^{242}$$Pu. Finally, the prepared spike was validated by parallel analysis of simulated sample of dissolved MOX solution. This spike was applied to measure the uranium and plutonium amount content of dissolved MOX solutions using isotope dilution mass spectrometry.

JAEA Reports

Preparation of Zr-91 stable isotope standard solution for determination of Zr-93 by mass spectrometry

Konda, Miki; Asai, Shiho; Hanzawa, Yukiko; Magara, Masaaki

JAEA-Technology 2015-054, 22 Pages, 2016/03


Isotope dilution mass spectrometry (IDMS) with ICP-MS is reliable method for determination of Zr-93, which is one of the long-lived fission products found in spent nuclear fuel and high-level radioactive wastes. In order to use an isotope standard solution of zirconium as the spike for IDMS, dissolving a commercially available solid isotope standard is indispensable. Prior to the dissolution of the Zr-91 isotope standard, solubility of metal zirconium in a mixture of HNO$$_3$$ and HF was evaluated using zirconium metal chips. Then, 2 mg of the Zr-91 isotope standard was dissolved with 0.2 mL of 1 M HNO$$_3$$-3 v/v% HF mixed solution, followed by adjusting the concentration of Zr-91 to approximately 1,000 $$mu$$g/g. IDMS, in which a natural isotopic abundance standard solution of zirconium was used as the spike, was employed for the determination of the concentration of Zr-91 in the prepared Zr-91 isotope standard solution. The concentration of Zr-91 in the prepared Zr-91 isotope standard solution was (9.6$$pm$$1.0) $$times$$ 10$$^2$$ $$mu$$g/g, which is in good agreement with the predicted concentration. This indicates that the Zr-91 metal isotope standard was completely dissolved with sufficient chemical stability. Additionally, no impurities were detected in the prepared Zr-91 isotope standard solution. These positive results denote that the Zr-91 isotope standard solution with the preferable quality for IDMS of Zr-93 can be obtained by the proposed dissolution procedures.

JAEA Reports


PNC TN8600 91-001, 68 Pages, 1991/02


no abstracts in English

Oral presentation

Reflection of domestically applied measurement method to the ISO 8299

Sumi, Mika; Suzuki, Toru

no journal, , 

JAEA's Plutonium Fuel Development Center (JAEA-PFDC) has established analysis procedure for the Isotope Dilution Mass Spectrometry (IDMS), which is applied for the accountancy analysis. Report on this procedure and actions to reflect those method to the international standard (ISO 8299).

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