• Title/Summary/Keyword: 열이온화 질량분석기

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동위원소희석법과 열이온화 질량분석기에 의한 화강암질 대수층내 지하수의 희토류원소 분포도 및 그 의의

  • 이승구;김건한;김용제;성낙훈;아키마사마스다
    • Proceedings of the Korean Society of Soil and Groundwater Environment Conference
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    • 2003.04a
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    • pp.59-62
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    • 2003
  • 동위원소희석법에 의한 열이온화 질량분석법 (ID-TIMS)을 이용하여 지하수내 희토류원소의 함량을 측정하였다. 희토류원소의 분리에는 철공침법과 양이온교환수지에 의한 컬름분리법을 이용하였다. 경희토류(La-Eu)와 Gd, Dy, Er의 경우 수-수십 ppt의 수준에서 1%이내의 오차범위를 측정되어졌으며, 중희토류 중 Yb와 Lu은 정확도가 다소 떨어진 10% 전후에서 측정되었다. 지하수내 함량을 운석으로 규격화한 결과, 경희토류가 부화되었고 중희토류는 결핍되었으며 Eu의 이상은 거의 존재하지 않는다. 특히 경희토류에서는 M-type의 테트라드효과, 중희토류에서는 W-type의 테트라드효과가 관찰되었다. 이는 희토류원소의 수화수와 밀접한 관련이 있는 것으로 사료된다.

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지하수와 강우내 희토류원소 분포도 및 지구화학적 의의

  • 이승구;김용제;김건한;성낙훈;박원배
    • Proceedings of the Korean Society of Soil and Groundwater Environment Conference
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    • 2003.09a
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    • pp.210-212
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    • 2003
  • 동위원소희석법에 의한 열이온화 질량분석법(ID-TIMS)을 이용하여 한국지질자원연구원과 에너지기술연구 원내 지하수와 강우 희토류원소의 함량을 측정/해석하였다. 분석결과를 토대로 지하수의 희토류원소 함량은 강우의 함량과 비교해 볼 때, 상대적으로 낮은 값을 보여준다. 그리고 굴착 심도가 더 깊은 한국지질자원연구원의 지하수내 희토류원소 함량이 한국에너지기술연구원의 지하수내 함량보다 더 낮은 값을 보여준다. 이는 강우가 지하로 흘러들어 가면서, 희토류원소와 대수층 구성암석과의 흡착반응에 의해 심부로 갈수록 함량이 낮아졌을 가능성이 크다고 판단된다. 뿐만 아니라, 강우의 경우, 희토류원소의 W형-테트라드 효과가 매우 현저하게 나타나고, 지하수에서는 M형과 W형의 테트라드 효과가 동시에 존재하는 특성이 강한데, 이는 희토류원소의 수화수 및 화강암 대수층과의 물-암석 반응에 의한 결과인 것으로 사료된다.

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Abundane of Rare Earth Element in Duwon Meteorite and Its Geochchemical Significance (두원운석의 희토류원소 존재도 및 지구화학적 의의)

  • Lee Seung-Gu;Kim Kun-Han;Choi Byeon-Gak
    • The Journal of the Petrological Society of Korea
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    • v.13 no.4
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    • pp.238-243
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    • 2004
  • Duwon meteorite was fallen on 23 November 1943 in Duwonmyeon, Goheung, Jeolanam-Do. We measured rare earth element abundance of Duwon meteorite by isotope dilution thermal ion mass spectrometry (ID-TIMS) and ICP-MS. As a result, except La and Ce, abundance of other rare earth element show a correspondence within 10% of error range. However, La and Ce show more than 70% in abundance, which is considered due to 1) experimental procedure or 2) inhomogeneity of sample. Leedey meteorite was fallen on 25 November 1943 in Dewey County, Oklahoma, USA. which suggested that fallen difference between Leedey and Duwon meteorites is only 2 days. Leedey and Duwon meteorites are classified as ordinary chondrite of L6 type. In Leedey chondrite-normalized REE pattern, Duwon meteorite shows nearly flattened, which suggests close relationship between Leedey and Duwon meteorites meteoritically or cosmochemically.

Optimal Conditions for Pretreated Sample for Sr Isotope Analysis by MC-ICP-MS: A Comparison Between Eichrom (SR-R50-S)'s and Bio-Rad(AG®50W-X8)'s Resins (다검출기 유도결합 플라즈마 질량분석기에 의한 Sr 동위원소 분석을 위해 전처리된 시료의 최적 조건: Eichrom사 Sr 수지(SR-R50-S)와 Bio-Rad사 수지(AG®50W-X8) 비교)

  • Myoung Jung, Kim;Seung-Gu, Lee
    • Korean Journal of Mineralogy and Petrology
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    • v.35 no.4
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    • pp.507-520
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    • 2022
  • The Sr isotope ratio, which is used as basic data for rock formation time, crustal and mantle evolution studies, is determined by mass spectrometer such as thermal ionization mass spectrometry (TIMS) or multi-detector inductively coupled plasma mass spectrometry (MC-ICP-MS). In this technical report, we compared how incomplete chemical separation of elements affects the determination of Sr isotope ratios. For the experiment, commercial resin, NBS987(NIST SRM987) Sr isotope standard, and rock standard samples from the Geological Survey of Japan (GSJ) such as JG1a, JB3 and JA1 were used. As a result of the comparative experiment, it was clearly observed that the measured values of 87Sr/86Sr change when Rb remains due to incomplete separation of the NBS987 Sr isotope standard sample as well as the rock standard samples of GSJ. This indicates that complete separation is an important factor since the calculated value deviates from the true value even though correction for isotope interference by isobar is performed when measuring the isotope ratio with MC-ICP-MS. This also suggests that, when reporting the measurement result of Sr isotope ratio using MC-ICP-MS, the measurement strength of 85Rb should be reported together with the measurement strength of all isotopes of Sr so that isotope interference by isobar can be judged.

The Study of Age Determination Using Stepwise Dissolution Technique (단계적 용해에 의한 연대측정법 연구)

  • 박계헌
    • The Journal of the Petrological Society of Korea
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    • v.10 no.3
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    • pp.133-147
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    • 2001
  • Recently developing method of age determination using stepwise dissolution technique to expand the applicability of absolute age determination significantly is evaluated whether it is applicable to the Korean samples. The materials selected for the study are uranium-bearing black slates from Changni Formation of Ogcheon metamorphic belt, tourmaline separated from Naedeongni granite of Yeongnam massif, garnet and ilmenite separated from ilmenite-bearing anorthositic rock of Yeongnam massif, scheelites from Ogbang mine, and magnetite separated from Gyemyeongsan Formation of Ogcheon metamorphic belt. For the stepwise dissolution, various acid steps with different normalities and different durations were applied to leach the samples. The leachate from each step was analyzed to determine the Pb isotopic composition and concentrations of Pb and U using thermal ionization mass spectrometer. The black slates from the Changni Formation and the tourmaline from the Naedeongni granite reveal significant variation of Pb isotopic composition, which reveals the potential of such stepwise dissolution technique as a dating method. The behaviors of uranium and lead during the each stage of step leaching are different, which seem to reflect the differences in positions within the crystal lattices depending upon mineral species.

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The isobaric effect on the measurement of Gd isotopes by thermal ionization mass spectrometry (열이온화 질량분석기를 이용한 Gd 동위원소 측정에서 동중원소 영향)

  • Jeon, Young-Shin;Park, Jong-Ho;Joe, Kih-Soo;Han, Sun-Ho;Song, Kyuseok
    • Analytical Science and Technology
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    • v.22 no.5
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    • pp.415-421
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    • 2009
  • A study was performed to investigate the isobaric effects of impurities in isotope measurement of gadolinium by TIMS. Especially, the ratio of $^{155}Gd/^{158}Gd$ showed the higher value than that of natural gadolinium and also decreased as the measuring time increased. This phenomenon is considered to be due to the oxide form of La ($LaO^+$, m/z=155) causing to create a serious bias on the measurement of $^{155}Gd$ abundance by La as an impurity, and due to $LaO^+$ produced more than the $Gd^+$ in the early time which disappears as the time goes on because of lower melting point and ionization potential of La than Gd. Although isobaric effects from Ba($BaO^+$), Ce($CeO^+$), Sm($SmO^+$), La($LaO^+$), and $K_4{^+}$(m/z=156)-cluster were detected even when blank rhenium filaments were used, these could be avoided by preconditioning(baking out) the filament. And we found that the measurement of $GdO^+$ instead of $Gd^+$ is more suitable in avoiding the isobaric effect from impurities such as La, Ce and Ba in the measurement of Gd isotope only in case of absence or extremely low level of Yb, Sm, Dy, Er, Lu.

Background effect on the measurement of trace amount of uranium by thermal ionization mass spectrometry (열이온화 질량분석에 의한 극미량 우라늄 정량에 미치는 바탕값 영향)

  • Jeon, Young-Shin;Park, Yong-Joon;Joe, Kih-Soo;Han, Sun-Ho;Song, Kyu-Seok
    • Analytical Science and Technology
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    • v.21 no.6
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    • pp.487-494
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    • 2008
  • 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.