# 열이온화 질량분석에 의한 극미량 우라늄 정량에 미치는 바탕값 영향

• Accepted : 2008.11.05
• Published : 2008.12.25
• 88 36

#### Abstract

An experiment was performed for zone refined Re-filament and normal (nonzone refined) Re-filament to reduce the background effect on the measurement of low level uranium samples. From both filaments, the signals which seemed to come from a cluster of light alkali elements, $(^{39}K_6)^+$, $(^{39}K_5+^{41}K)^+$ and $PbO_2$ were identified as the isobaric effect of the uranium isotopes. The isobaric effect signal was completely disappeared by heating the filament about $2000^{\circ}C$ at < $10^{-7}$ torr of vacuum for more than 1.5 hour in zone refined Refilaments, while that from the normal Re-filaments was not disappeared completely and was still remained as 3 pg. of uranium as the impurities after the degassing treatment was performed for more than 5 hours at the same condition of zone refined filaments. A threshold condition eliminating impurities were proved to be at 5 A and 30 minutes of degassing time. The uranium content as an impurity in rhenium filament was checked with a filament degassing treatment using the U-233 spike by isotope dilution mass spectrometry. A 0.31 ng of U was detected in rhenium filament without degassing, while only 3 pg of U was detected with baking treatment at a current of 5.5 A for 1 hr. Using normal Re-filaments for the ultra trace of uranium sample analysis had something problem because uranium remains to be 3 pg on the filament even though degassed for long hours. If the 1 ng uranium were measured, 0.3% error occurred basically. It was also conformed that ionization filament current was recommended not to be increased over 5.5 A to reduce the background. Finally, the contents of uranium isotopes in uranium standard materials (KRISS standard material and NIST standard materials, U-005 and U-030) were measured and compared with certified values. The differences between them showed 0.04% for U-235, 2% for U-234 and 2% for U-236, respectively.

#### Keywords

Uranium isotope;thermal ionization mass spectrometer;background test;rhenium filament

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#### Acknowledgement

Supported by : 교육과학기술부