• Title/Summary/Keyword: thermal ionization mass spectrometry

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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.

A Study of the Microstructure and Provenance Area of Bronze Spoons Excavated from the Ok-dong Site in Andong (안동 옥동유적 출토 청동시(靑銅匙)의 미세조직 및 산지연구)

  • Chung, Kwang-Yong;Lee, Joo-Hyun
    • Journal of Conservation Science
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    • v.25 no.4
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    • pp.411-420
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    • 2009
  • A series of scientific analyses, including ICP-AES, microstructure, and TIMS, were carried out on 5 bronze spoons among 14 bronze artifacts excavated from the Ok-dong site in Andong, North Gyeongsang Province. The results of analysis showed that the bronze spoons were formed from an alloy of no more than 75% Cu and 21~23% Sn, placing it in the category of brassware, with trace elements such as Pb, Fe, and Zn. In particular, plumbum Pb contents of which traces of 0.04% were found, appears to have been added as an impurity during smelting. The microstructure of the bronze spoons suggests that the casting process involved using a spoon-shaped hollow mold, followed by an ropid-cooling process after the shape was perfected at approximately $586^{\circ}C$. After comparison of data measured from thermal ionization mass spectrometry (TIMS) of galena from Korea, China, and Japan, it appears that the raw materials for the bronze spoons included galena (lead sulfide) produced from the southern part of China.

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Rb-Sr Isotopic Ages of Biotite in the Weathering Profile of Granodiorite, Yecheon (예천지역 화강섬록암 풍화대내 흑운모의 Rb-Sr 동위원소연대 변화)

  • Jeong Gi Young;Cheong Chang-Sik;Lee Bong Ho
    • Journal of the Mineralogical Society of Korea
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    • v.18 no.1
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    • pp.53-59
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    • 2005
  • Rb-Sr isotopic ages of oxidized biotite in the weathering profile of granodiorite, Yecheon area, were measured by thermal ionization mass spectrometry, and compared with their K-Ar ages. A decrease of Rb-Sr isotopic age is well correlated with iron oxidation, and consistent with K-Ar age. Octahedral and interlayer cations including Rb and Sr were partly released from the oxidizing biotite by excess positive charge from iron oxidation. Divalent /sup 87/Sr decayed from monovalent /sup 87/Rb was more easily released from biotite, resulting in the reduction of Rb-Sr isotopic age. Weathered biotite is not suitable for the age dating of parent rocks, but behaviour of radiogenic isotopes provides useful information on the geochemical and structural changes of biotite during weathering.

Provenance Analysis of Horse-shaped Bronze Buckles Excavated from Site of Songjeol-dong, Cheongju (납동위원소비 분석을 활용한 청주 송절동유적 출토 마형대구의 원료산지 고찰)

  • Bae, Go Woon;Lee, Sang Ok;Chung, Kwang Yong;Shin, Seoung Chul
    • Journal of Conservation Science
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    • v.35 no.3
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    • pp.209-216
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    • 2019
  • Lead isotope ratios in horse-shaped bronze buckles excavated from the Songjeol-dong site in Cheongju and the mid-western region of the Korean Peninsula have been determined by thermal ionization mass spectrometry. The lead isotope ratios of the samples with data provenance were plotted in zone 3 of the South Korean galena map. The results indicated that the horse-shaped bronze buckles could be made using galena located in the same area as the archaeological site. These results can be used as basic data for comparison purposes in future studies on the manufacturing technology and provenance of bronze artifacts.

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.