• Mass Spectrometry Letters
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• 제7권3호
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• pp.64-68
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• 2016

Scanning electron microscopy combined with thermal ionization mass spectrometry (SEM-TIMS) was used to determine the precise isotope ratios of ultra-trace levels of uranium contained in individual microparticles. An advanced multiple ion counter system consisting of three secondary ion multipliers and two compact discrete dynodes was used for complete simultaneous ion detection. For verification purposes, using TIMS with complete simultaneous measurement, isotopes were analyzed in 5 pg of uranium of a certified reference material. A microprobe in the SEM was used to transfer individual particles from a NUSIMEP-7 sample to TIMS filaments, which were then subjected to SEM-TIMS and complete simultaneous measurement. The excellent agreement in the resulting uranium isotope ratios with the certified NUSIMEP-7 values shows the validity of SEM-TIMS with complete simultaneous measurement for the analysis of uranium isotopes in individual particles. Further experimental study required for investigation of simultaneous measurement using the advanced multiple ion counter system is presented.

• 분석과학
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• 제23권6호
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• pp.518-523
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• 2010

본 논문에서는 반응속도론적 인광 분석기(Kinetic Phosphorescence Analyzer, KPA)를 이 용하여 환경 시료 중의 우라늄 동위원소 분석에 대한 연구를 기술하였다. 극초단파 산분해 기술을 이용하여 토양 및 유리 재질 시료로부터 우라늄 성분을 추출한 후, UTEVA 수지를 통해서 우라늄 동위원소를 순수하게 분리하였고 KPA로 우라늄 농도를 정량하였다. 우라늄 표준용액을 사용하여 KPA를 이용한 우라늄 측정법에 대한 선형성 및 재현성 실험을 수행하였다. 우라늄 표준용액, 지하수 및 인증 표준시료에 대해 KPA를 사용하여 우라늄 농도를 측정하여 KPA를 이용한 우라늄 분석법에 대한 신뢰도를 검증하였다.

• Journal of Radiation Protection and Research
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• 제26권1호
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• pp.1-6
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• 2001

방사성 동위원소에 오염된 토양시료에 대하여 정확하고 신속한 U 등위원소 분석법을 개발하였고 IAEA 표준시료에 적용하여 분석법의 타당성을 검증하였다. TBP 용매추출법의 단점을 보완하기 위해서 토양시료를 질산 및 불산을 사용하여 메트릭스 성분으로부터 우라늄을 완벽하게 추출하였고 이온교환수지와 TRU Spec 수지를 이용하여 우라늄 등위원소를 악티나이드 원소로부터 순수분리하였다. 크로마토 그래피 추출법을 사용하여 토양시료에서 우라늄 등위원소 화학수율은 TBP 용매추출법의 경우보다 10% 정도 증가하였다. 크로마토 그래피 추출법을 사용한 IAEA 토양시료에 분석결과는 IAEA에서 보고된 수치와 일치하였다.

• 분석과학
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• 제31권3호
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• pp.134-142
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• 2018

The uranium isotopic ratio in environmental samples around nuclear facilities is important because it reveals information regarding illegal activities or anthropogenic pollution. Determination of uranium isotopes, however, is a challenging task requiring much labor and time because of the complex separation procedures and lengthy process. In this study, a rapid determination method for uranium isotopes in environmental samples was developed using. The sample was completely decomposed using the alkali fusion method. The separation procedure using extraction chromatography (UTEVA) was simplified in a single step without any further removal process for Si and major matrix elements. The established method can be completed within 3 h from sample dissolution to ICP-MS measurement. Most matrix elements and uranium isotopes in the soil samples were well separated and purified. Five types of were used to assess the method's accuracy and precision for a rapid uranium analysis method. The analytical accuracy for all CRM samples ranged from 95.1 % to 97.8 %, and the relative standard deviation was below 3.9 %. From the analytical results, one may draw conclusions that the evaluated method for uranium isotopes using alkali-fusion, the extraction chromatography process, and ICP-MS measurements is fast and fairly reliable owing to its recovering efficiencies. Thus, it is expected that the evaluated method can contribute to the improvement of environmental monitoring ability.

• Mass Spectrometry Letters
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• 제3권2호
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• pp.54-57
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• 2012

Mass spectrometric analysis was carried out using multicollector inductively coupled plasma mass spectrometry (MC-ICP-MS) for the precise and accurate determination of the isotope ratios of ultratrace levels of uranium dissolved in 3% $HNO_3$. We used the certified reference material (CRM) 112-A at a trace level of 100 pg/mL for the uranium isotopic measurement. Multiple collectors were utilized for the simultaneous measurement of uranium isotopes to reduce the signal uncertainty due to variations in the ion beam intensity over time. Mass bias correction was applied to the measured U isotopes to improve the precision and accuracy. Furthermore, elemental standard solution with certified values of platinum, iridium, gold, and thallium dissolved in 3% $HNO_3$ were analyzed to investigate the formation rates of the polyatomic ions of $Ir^{40}$ $Ar^+$, $Pt^{40}$ $Ar^+$, $Tl^{40}$ $Ar^+$, $Au^{40}$ $Ar^+$ for the concentration range of 50-400 pg/mL. Those polyatomic ions have mass-to-charge ratios in the 230-245 m/z region that it would contribute to the increase of background intensity of uranium, thorium, plutonium, and americium isotopes. The effect of the polyatomic ion interference on uranium isotope measurement has been estimated.

• Nuclear Engineering and Technology
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• 제50권1호
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• pp.140-144
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• 2018

Isotopic analyses of plutonium and low-enriched uranium mixtures with particle sizes of $0.6-3.3{\mu}m$ were performed using thermal ionization mass spectrometry with a continuous heating method to verify its effectiveness for the accurate analysis of minor isotopes without sample pretreatment. The mixed particles used in this study were prepared from a mixed solution of plutonium (SRM 947) and uranium (U010, $^{235}U$ 1% enriched) reference materials. The isotope ratios for plutonium in the individual mixed particles, including $^{238}Pu/^{239}Pu$, $^{241}Pu/^{239}Pu$ as well as $^{240}Pu/^{239}Pu$, and $^{242}Pu/^{239}Pu$, were in good agreement with the certified values despite the isobaric interference of $^{238}U$ and $^{241}Am$. The isotope ratios for uranium in the mixed particles also agreed well with the certified values within the range of error. However, the isotope ratios for minor isotopes, such as $^{234}U$ and $^{236}U$, in the particles with diameters of less than approximately $1.8{\mu}m$ could not be measured because numbers of $^{234}U$ and $^{236}U$ atoms in analyzed particles are too low. These results indicate that thermal ionization mass spectrometry with a continuous heating method is applicable for the analysis of trace amounts of plutonium isotopes, including $^{238}Pu$ and $^{241}Pu$, despite the presence of the respective isobars $^{238}U$ and $^{241}Am$ in the microsamples.

• Bulletin of the Korean Chemical Society
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• 제32권12호
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• pp.4327-4331
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• 2011

A new method in thermal ionization mass spectrometry (TIMS) was developed to correct peak tailing backgrounds in the isotope ratio measurements of uranium in ultra trace levels for higher accuracy. Two different uranium standard reference materials (U005 and U030) were used to construct databases of signal intensities at mass 234 u and mass 236 u, which correspond to the two uranium minor isotopes, and signal intensity of $^{238}U$. Correlations between peak tailing backgrounds and $^{238}U$ were obtained by least-squares regression on calculated backgrounds at mass 234 u and mass 236 u with respect to the signal intensity of $^{238}U$ followed by separation of the peak tails of the two major isotopes of uranium ($^{235}U$ and $^{238}U$), which enables us to obtain a master equation for peak tailing background correction on all kinds of samples. Verification of the correction method was carried out using U010 and IRMM-040a.

• Mass Spectrometry Letters
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• 제4권3호
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• pp.51-54
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• 2013

Isotopic analysis using thermal ionization mass spectrometry coupled with scanning electron microscopy (SEM-TIMS) was performed to determine the isotopic ratios of uranium contained in micro-particles in the 6th Nuclear Signatures Interlaboratory Measurement Evaluation Programme (NUSIMEP-6) sample. Elemental analysis by energy dispersive X-ray spectroscopy (EDS) was conducted on uranium-bearing mirco-particles, which were transferred to rhenium filaments for TIMS loading using a micromanipulation system in a SEM. A multi-ion-counter system was utilized to detect the ion signals of the four isotopes of uranium simultaneously. The isotope ratios of uranium corrected by bracketing using a reference material showed excellent agreement with the certified values. The measurement accuracy for $n(^{234}U)/n(^{238}U)$ and (b) $n(^{235}U)/n(^{238}U)$ was 10% and 1%, respectively, which met the requirements for qalification for the NetWork of Analytical Laboratories (NWAL).

• Nuclear Engineering and Technology
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• 제31권5호
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• pp.445-454
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• 1999

This work describes the adaptation of extractive scintillation by URAE $X^{TM}$ with a photon-electron rejecting alpha liquid scintillation (PERAL $S^{)}$ spectrometer to the analysis of uranium in aqueous samples. The extraction efficiency of the system was evaluated under varing chemical conditions including pH, and sample-cocktail volume ratio. Isotopic information from the (PERAL $S^{)}$ spectrum of natural uranium was obtained using a curve fitting routine. Comparisons of the result with that obtained from alpha spectrometry method using ion implanted silicon detector showed good agreement.t.

• Nuclear Engineering and Technology
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• 제29권4호
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• pp.327-335
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• 1997

The correlation of isotope composition of uranium, plutonium and neodymium with the burnup in M uranium dioxide fuel has been investigated experimentally. The total and fractional($^{235}$ U) burnup were determined by Nd-148 and, U and Pu mass spectrometric method respectively. The isotope compositions of these elements, after their separation from the fuel samples were measured by mass spectrometric. The content of the elements in the irradiated fuel ore determined by isotope dilution mass spectrometric method using $^{233}$ U, $^{242}$ Pu and $^{150}$ Nd as spikes. The content of plutonium in the irradiated fuel was expressed by the correlation with uranium isotopes. The correlations between isotope compositions themselves and the total and fractional burnup ore compared with those calculated from ORIGEN2 code.