量研学術機関リポジトリ「QST-Repository」は、国立研究開発法人 量子科学技術研究開発機構に所属する職員等が生み出した学術成果（学会誌発表論文、学会発表、研究開発報告書、特許等）を集積しインターネット上で広く公開するサービスです。 Welcome to QST-Repository where we accumulates and discloses the academic research results(Journal Publications, Conference presentation, Research and Development Report, Patent, etc.) of the members of National Institutes for Quantum Science and Technology.
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Two fusion methods were established for rapid determination of Pu in soil and sediment samples. The methods consisted of NH4HSO4 or NH4HF2 fusion procedures incorporated with procedures for CaF2/LaF3 co-precipitation, extraction chromatography and SF-ICP-MS measurement. The fusion procedures were done at 250oC on a portable hot plate instead of in a cumbersome muffle furnace and took only 15 min. Chemical recoveries of Pu after completing the NH4HSO4 and NH4HF2 fusion methods for 0.5-1 g sample were approximately 70% and more than 90%, respectively, and decreased with the increase of sample weight from 0.5 g to 5 g. Sediment samples were pre-ignited at different temperatures ranging from 450 oC to 1000 oC to form refractory fractions of Pu, with which the dissolution rates of Pu by the NH4HSO4 and NH4HF2 fusion were investigated. With the increase of pre-ignition temperature of the sediment samples, the dissolution rates of Pu from the samples prepared by NH4HSO4 fusion declined dramatically from near 100% for 450 oC to 8% for 1000 oC. In contrast, the NH4HF2 fusion was capable of completely releasing Pu from samples that were pre-ignited at temperatures over 450 oC to 1000 oC, which was comparable to releases obtained by the hazardous and time-consuming HNO3-HF digestion, and was superior to the conventional HNO3 digestion. Additionally, because HF is not used in any procedure of the NH4HF2 fusion, a safer and greener alternative to NH4HSO4 fusion and HNO3-HF digestion is realized for rapid Pu determination in environmental samples for nuclear emergency response and application in environmental studies.
Low-temperature fusion using NH4HSO4 and NH4HF2 for rapid determination of Pu in soil and sediment samples
