• 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.

• Communications for Statistical Applications and Methods
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• 제8권1호
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• pp.51-63
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• 2001

We are interested in the conditional independence in sparse $2\tims2\tims$K tables with very rare cell counts. The most popular test is Cochran-Mantel-Haenszel statistic when sample sizes are moderately large enough to guarantee the chi-square approximation. We will consider jackknifing the CMH test and also suggest an approximate normal distribution for the standardized jackknifed CMH statistic. The main focus of this paper is to improve the chi-squared approximation to the CMH test by using the asymptotic normality of the jackknifed CMH test when sample sizes are very sparse but K and N$\infty$. The performance of the proposed jackknifed test, in the sense of significance level control and power, will be compared with that of the CMH test through a Monte Carlo study.

• Journal of Radiation Protection and Research
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• 제43권3호
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• pp.120-123
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• 2018

Background: Analysis of enrichment of $UO_2$ is important to verify the information declared by the license-holders. The redundancy methods are required to guarantee the analysis result. Korea Institute of Nuclear Nonproliferation and Control (KINAC) used to analyze it with alpha spectrometry and consign to Korea Basic Science Institute (KBSI) Thermal Ionization Mass Spectrometry (TIMS). This article evaluated the similarity of the results with two methods and derive correlation equation. It could be compared to the results measured by TIMS running by KBSI. Materials and Methods: There are not many certified materials for the uranium enrichment value. Therefore, 34 uranium pellets, which have the wide range of uranium enrichment from 0.21 to 4.69 wt%, were used for the experiments by the alpha spectrometry and the TIMS. Results and Discussion: The study shows there are the tendency of analyzed enrichment by each equipment. It shows uranium enrichment with alpha spectrometry evaluated 17% higher than that with TIMS on average. The regression equations were also derived in case the similarity between the two results with two methods is lower than predicted. Two experiments were designed to compare the effect of number of samples. The $R^2$ was 0.9977 with 34 pellets. It shows the equation is appropriate to predict the enrichment values by TIMS with that of alpha spectrometry. The $R^2$ was 0.9858 with four pellets for ten times. The $R^2$ decreased while the number of samples increased. The discrepancy between the lowest and highest enrichment seems to be one of the reason for it. Conclusion: KINAC expects the first equation with 34 samples is useful to predict the result with TIMS, the redundancy method, based on the alpha spectrometry. The extra samples are necessary to collect if the enrichment value analyzed by TIMS is lower than the value predicted with the equation. Further study would be followed related to the impact of the peak counts for each uranium isotopes, sample amount and number of experiments when TIMS established in KINAC by the end of 2018.

• Mass Spectrometry Letters
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• 제2권2호
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• pp.57-60
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• 2011

As background significantly affects measurement accuracy and a detection limit in determination of the trace amounts of uranium, it is necessary to determine the impurities in the Lexan detector film for single particle measurements by thermal ionization mass spectrometry coupled with fission track technique (FT-TIMS). We have prepared various micro sizes of the blank Lexan detector film using a micromanipulation technique for uranium measurements by TIMS. Few tens of fg of uranium background with no remarkable dependency on the film sizes were observed in the blank Lexan films with the sizes from $50{\times}50\;{\mu}m^2$ to $300{\times}300\;{\mu}m^2$. Based on the determination of the uranium background in the Lexan film, any background correction is necessary in the isotopic analysis of a uranium single particle with micron sizes when the particle bearing Lexan film is dissected with less than $300{\times}300\;{\mu}m^2$ size. The isotopic analysis of a uranium particle in U030 standard material using TIMS was carried out to verify the applicability of the Lexan film to the single particle analysis with high accuracy and precision.

• Mass Spectrometry Letters
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• 제7권4호
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• pp.102-105
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• 2016

This study explored the feasibility of using a carburization technique to enhance the ion intensity of isotopic analysis of ultra-trace levels of uranium using thermal ionization mass spectrometry (TIMS). Prior to fixing uranium samples on TIMS filaments, graphite powder suspended in nitric acid was deposited on rhenium filaments. We observed an enhancement of $^{238}U^+$ intensity by a factor of two when carburization was used, and were able to roughly optimize the amount of graphite powder necessary for carburization. The positive shift in heating current when evaporating filaments upon carburization implies that uranium was chemically altered by carburization, when compared to normal fixation processes. The good agreement between our method and known standards down to an ultra-trace level shows that the proposed technique can be applied to isotopic uranium analysis down to abundances of ~10 pg.

• Mass Spectrometry Letters
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• 제5권1호
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• pp.12-15
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• 2014

Thermal ionization mass spectrometry (TIMS) was used to determine the concentration and isotope ratio of uranium contained in samples of soil and groundwater collected from Korea. Quantification of uranium in ground water samples was performed by isotope dilution mass spectrometry. A series of chemical treatment processes, including chemical separation using extraction chromatography, was applied to the soil samples to extract the uranium. No treatments other than filtration were applied to the groundwater samples. Isotopic analyses by TIMS showed that the isotope ratios of uranium in both the soil and water samples were indistinguishable from those of naturally abundant uranium. The concentration of uranium in the groundwater samples was within the U.S. acceptable standards for drinking water. These results demonstrate the utility of TIMS for monitoring uranium in environmental samples with high analytical reliability.

• 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).

• 정보관리연구
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• 제30권3호
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• pp.55-72
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• 1999

산업기술정보원이 자체 개발한 사내 정보관리시스템인 TIMS의 구성과 주요특징, 제공기능 등에 대하여 설명하고, TIMS를 활용한 기업의 정보관리모델을 제시함으로써 기업의 정보관리 활동에 도움을 주고자 하였다.

• Mass Spectrometry Letters
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• 제1권1호
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• pp.17-20
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• 2010

As background significantly affects measurement accuracy and a detection limit in determination of the trace amounts of uranium, it is necessary to minimize the impurities in the filaments used for thermal ionization mass spectrometry (TIMS). We have varied the degassing condition such as the heating currents and duration times to reduce the backgrounds from the filaments prepared with zone-refined rhenium tape. The most efficient degassing condition of the heating current and the duration time was determined as 3.5 A and 60 min, respectively. The TIMS measurement combined with the isotope dilution mass spectrometry (IDMS) technique showed that the uranium backgrounds were determined to be in a few fg level from blank rhenium filaments. The background minimized filaments were utilized to measure the uranium isotope ratios of a U030 (NIST) standard sample. The excellent agreement of the measurement with the certified isotope ratios showed that the degassing procedure optimized in this study efficiently reduced the impurity signals of uranium from blank rhenium filaments to a negligible level.

• 암석학회지
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• 제10권3호
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• pp.157-171
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• 2001

다검출기 유도결합 플라즈마 질량분석기(Multi-Collector Inductively Coupled Plasma Mass Spectrometer; MC/ICP/MS; AXIOM MC 모델)를 이용한 Pb동위원소 분석 시 고려 사항인 Pb/Ti 비율, Pb농도 영향, 기질 원소 영향을 살펴보고, NBS 981 용액을 2001년 3월부터 8월까지 42번 측정하여 정확도 및 재현성 을 검토하였다. 그리고 암석, 청동기 및 퇴적물 시료의 Pb 동위원소를 분석하여 열 이온화 질량분석기(TIMS) 자료와 비교하였다. NBS 981 Pb 200 ng으로 동위원소 비율을 측정하였을 때 $^{206}$ $Pb^{204}$ , $Pb^{207}$ //$Pb^{204}$ , $Pb^{208}$ $Pb^{204}$ Pb 비율은 약 500 ppm(2sd), $^{/}$$207^{206}$ Pb 및 $Pb^{208}$ $Pb^{206}$Pb 비율은 100~200 ppm(2sd)의 재현성을 얻을 수 있었다. Pb등위원소 분석의 정확도 및 재현성 측면에서 최적 조건은 1) Pb/Tl농도 비가 10 이고 2) Pb농도가 100 ng/ml 이상이며 3) 질량 분별 효과는 지수 법칙에 따라 보정하고 이 때 사용된 Tl의 동위원소 비율($^{205}$ $Tl^{203}$ Tl)은 2.3887이며 질량 분별 인자는 측정된 $208^{Pb}$ $^{206}$ 및 $Pb^{205}$ $Tl^{203}$ Tl 비율로부터 경험적으로 구해진 Pb의 인자를 이용하는 것이었다. 시료 중의 기질 원소들(matrix elements)에 의한 Pb 동위원소 비율의 영향은 없는 것으로 판단되며, TIMS와 비교된 시료들에 대하여 Pb 등위원소들은 측정 오차 범위 내에서 잘 일치하였다. 즉, MC/ICP/MS에 의한 Pb 동위원소 분석은 시료 전처리 단계를 줄여도 WS와 유사한 정밀도를 얻을 수 있어 신속한 분석방법이라 할 수 있다.다.