• Title, Summary, Keyword: MC-ICP-MS

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Rapid and Precise Determination of Pb Isotope Ratios Using Mu1ti-Collector ICP/MS (다검출기 유도결합 플라즈마 질량분석기를 이용한 신속하고 정밀한 Pb 동위원소 분석)

  • 최만식;정창식;신형선;임태선
    • The Journal of the Petrological Society of Korea
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    • v.10 no.3
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    • pp.157-171
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    • 2001
  • This study investigated the effects of Pb/Tl ratio, Pb concentration and concomitant matrix elements on the measurement of Pb isotope ratios using multi-collector ICP/MS (AXIOM MC model). Accuracy and reproducibility of Pb isotope ratios in NBS 981 solution were estimated for 42 data measured from March to August 2001. Pb isotopes measured in rocks, bronzes and sediments were compared to data measured by TIMS. Reproducibilities for $^{206}Pb/^{204}Pb,\; ^{207}Pb/^{204}Pb,\;and\;^{208}Pb/^{204}Pb$ ratio were about 500 ppm (2sd) and for $^{207}Pb/^{206}Pb$\;and\;^{208}Pb/^{206}Pb$ were 100~200 ppm for 200 ng of Pb in NBS 981 solution. The optimum conditions for the analysis of Pb isotope ratios with AXIOM MC for best accuracy and reproducibility were defined as follows; 1) Pb/Tl ratio is about 10 2) Pb concentration is about 100 ng/ml 3) correction for mass discrimination is performed by exponential law using 2.3887 of $^{205}Tl/^{203}Tl$ and Pb mass fractionation factor empirically obtained from $ln(^{208}Pb/^{206}Pb)-ln(^{205}Tl/^{203}Tl)$ relationship. The sample data measured with MC/ICP/MS for acid-digested and chemically separated rock samples, and acid-digested bronze samples and sediment samples coincide with those of TIMS within analytical errors. Therefore, MC/ICP/MS is a rapid analytical technique for Pb isotope ratios with the similar precision compared with TIMS.

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Improvement of Measurement Precisions for Uranium Isotopes at Ultra Trace Levels by Modification of the Sample Introduction System in MC-ICP-MS

  • Park, Ranhee;Lim, Sang Ho;Han, Sun-Ho;Lee, Min Young;Park, Jinkyu;Lee, Chi-Gyu;Song, Kyuseok
    • Mass Spectrometry Letters
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    • v.7 no.2
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    • pp.50-54
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    • 2016
  • Multi-collector inductively coupled plasma mass spectrometry (MC-ICP-MS) is currently used in our laboratory for isotopic and quantitative analyses of nuclear materials at ultra-trace levels in environmental swipe samples, which is a very useful for monitoring undeclared nuclear activities. In this study, to improve measurement precisions of uranium isotopes at ultratrace levels, we adopted a desolvating nebulizer system (Aridus-II, CETAC., USA), which can improve signal sensitivity and reduce formation of uranium hydride. A peristaltic pump was combined with Aridus-II in the sample introduction system of MC-ICP-MS to reduce long-term signal fluctuations by maintaining a constant flow rate of the sample solution. The signal sensitivity in the presence of Aridus-II was improved more than 10-fold and the formation ratio of UH/U decreased by 16- to 17- fold compared to a normal spray chamber. Long-term signal fluctuations were significantly reduced by using the peristaltic pump. Detailed optimizations and evaluations with uranium standards are also discussed in this paper.

Validation of Bulk Analysis with Simulated Swipe Samples Containing Ultra-Trace Amounts of Uranium and Plutonium Using MC-ICP-MS

  • Lim, Sang Ho;Han, Sun-Ho;Park, Jong-Ho;Park, Ranhee;Lee, Min Young;Park, Jinkyu;Lee, Chi-Gyu;Song, Kyuseok
    • Mass Spectrometry Letters
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    • v.6 no.3
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    • pp.75-79
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    • 2015
  • Suitable analytical procedures for the bulk analysis of ultra-trace amounts of uranium and plutonium have been developed using multi-collector inductively coupled mass spectrometry (MC-ICP-MS). The quantification and determination of the isotopic ratios of uranium and plutonium in three simulated swipe samples, a swipe blank, and a process blank were performed to validate the analytical performance. The analytical results for the simulated swipe samples were in good agreement with the certified values, based on the measurement quality goals for the analysis of bulk environmental samples recommended by the International Atomic Energy Agency (IAEA)

Accurate Measurement of Isotope Amount Ratios of Lead in Bronze with Multicollector Inductively Coupled Plasma Mass Spectrometry

  • Lee, Kyoung-Seok;Kim, Jin-Il;Yim, Yong-Hyeon;Hwang, Euijin;Kim, Tae Kyu
    • Mass Spectrometry Letters
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    • v.4 no.4
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    • pp.87-90
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    • 2013
  • Isotope amount ratios of lead in a bronze sample have been successfully determined using multicollector inductively coupled plasma mass spectrometry (MC-ICP-MS). Matrix separation conditions were tested and optimized using ion exchange chromatography with anion-exchange resin, AG1-X8, and sequential elution of the 0.5 M HBr and 7 M $HNO_3$ to separate lead from very high contents of copper and tin in bronze matrix. Mercury was also removed efficiently in the optimized separation condition. The instrumental isotope fractionation of lead in the MC-ICP-MS measurement was corrected by the external standard sample bracketing method using an external standard, NIST SRM 981 lead common isotope ratio standard followed by correction of procedure blank to obtain reliable isotope ratios of lead. The isotope ratios, $^{206}Pb/^{204}Pb$, $^{207}Pb/^{204}Pb$, $^{208}Pb/^{204}Pb$, and $^{208}Pb/^{206}Pb$, of lead were determined as $18.0802{\pm}0.0114$, $15.5799{\pm}0.0099$, $38.0853{\pm}0.0241$, and $2.1065{\pm}0.0004$, respectively, and the determined isotope ratios showed good agreement with the reference values of an international comparison for the same sample within the stated uncertainties

The Improved Method for Precise Determination of Pu Isotope Ratio using MC-ICP-MS (다중검출기유도결합플라즈마질량분석기를 이용한 Pu 동위원소비 정밀 분석법)

  • Yim, Seong-A;Han, Eun-Mi;Chae, Jung-Seok;Yun, Ju-Young
    • Journal of Radiation Protection and Research
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    • v.35 no.3
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    • pp.117-123
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    • 2010
  • Plutonium is by far the most important of the transuranic elements which have been released into the environment due to radio-toxicity and long term radiation effects on humans. And Pu isotope ratio ($^{240}Pu/^{239}Pu$) is of great interest because this ratio is used as a fingerprint for different sources. Mass spectrometry has been used as an useful atom counting technique with several advantages over decay counting techniques for the determination of Pu isotopes. It enables a determination of Pu isotope ratio in the environmental samples with a low detection limit and a short determination time. An ICP-MS is the representative mass spectrometry for Pu determination. In this study, the precision of $^{240}Pu/^{239}Pu$ isotope ratio was improved by using 4 multiple ion counters of MC-ICP-MS. The detection limit of $^{239}Pu$ and $^{240}Pu$ were $0.10\;fg\;ml^{-1}$ ($0.24\;{\mu}Bq\;ml^{-1}$), $0.12\;fg\;ml^{-1}$ ($0.97\;{\mu}Bq\;ml^{-1}$), respectively. The relative standard deviation of $^{240}Pu/^{239}Pu$ isotope ratio was less than 1 % in trace level. The various reference materials (seawater, soil and sediment) were analyzed to verify this method and their analytical results were in good agreement with the certified (or recommended value) value.

Improving Strontium Isotope Ratio Analysis Using MC-ICP-MS (다검출기 유도결합 플라즈마 질량분석기를 이용한 스트론튬 동위원소비 분석법 개선)

  • Lee, Sin-Woo;Park, Jaeseon;Park, Hyun-Woo;Hwang, Jong Yeon;Kim, Kumhee;Chung, Hyun-Mi;Choi, Jong-Woo
    • Journal of The Korea Society For Environmental Analysis
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    • v.21 no.4
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    • pp.237-242
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    • 2018
  • Strontium (Sr) commonly exists in rock, groundwater, soil, plants, and animals. The Sr isotope ratio offers important information as a tracer on nature because the Sr isotopic composition is not fractionated by any biological process in these ecosystems. Hence, Sr isotope ratio has been used in several studies on tracing the Sr source for contaminated sites and human migration. In this study, we developed a separation method for Sr content, and then improved Sr isotope analysis using multi-collector inductively coupled plasma mass spectrometry (MC-ICP-MS). A powdered rock standard (NIST 2710a) was used to determine the removal of interference elements (Rb and Ca) and the recovery rate of Sr content. The results ranged from 98% to 106%. Additionally, three standard samples (NBS 987, IAPSO and NIST 1486) were analyzed to evaluate the precision and accuracy of the results. The measured $^{87}Sr/^{86}Sr$ ratio for all the samples were consistent with the reported values, within an error. These results indicate that our established Sr separation and Sr isotope measurement methods are reliable and can hence be useful in the fields of environmental and forensic sciences.

Copper Isotope Measurements Using a Neptune MC-ICP-MS (다검출기 유도결합 플라즈마 질량분석기를 이용한 구리 동위원소 분석법)

  • Park, Sanghee;Ryu, Jong-Sik;Shin, Hyung Seon;Kil, Youngwoo;Jo, Yunsoo
    • Journal of the Mineralogical Society of Korea
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    • v.29 no.4
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    • pp.221-227
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    • 2016
  • Copper is an essential transition metal involving in various biogeochemical processes. With the recent advances in analytical techniques and mass spectrometry, such as MC-ICP-MS, it is possible to measure Cu isotopes, which allows us to understand various biogeochemical processes in detail. Nonetheless, few studies have been performed in South Korea. In this study, we compared two purification methods previously reported using an anion exchange resin ($AG^{(R)}$ MP-1M), developed the best method in our lab environment, and then verified it by measuring Cu isotopic compositions in two USGS geological reference materials (BHVO-2 and BIR-1a). Although all matrix cations causing mass bias were effectively removed through both two methods with the yield of better than 95%, the method using the mixture of HCl and $H_2O_2$ only displays Cu isotopic compositions, in excellent agreement with reported values within the error. The method developed in this study is expected to be commonly applied to earth and environmental sciences.

Molybdenum Isotope Analysis of Standard Reference Materials (표준물질을 이용한 몰리브덴 동위원소 분석)

  • Jo, Yunsoo;Kil, Youngwoo;Ryu, Jongsik;Seol, Junghwan;Nguyen, The Cong;Jung, Woochul;Park, Sanghee
    • Economic and Environmental Geology
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    • v.49 no.2
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    • pp.89-95
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    • 2016
  • Mo isotope, one of highly redox-sensitive isotopes, has been shown to be useful tracers of geochemical processes. Many studies for Mo isotope have documented with the help of recently developed analysis tools, but it has not yet been documented in the Korea. In this study, we introduce two-stage column separation method of Mo using column tube (BioRad PolyPrep(R) column, 10 ml) and anion exchange resin (BioRad Resin AG(R) 1-X8, 200-400 mesh). Mo isotope ratios in the solid SRMs (BHVO-2, SDO-1, PACS-2) and liquid SRM (IAPSO) were measured on MC-ICP-MS (Multi-collector Inductively Coupled Plasma Mass Spectrometer) and then compared with reference Mo isotope ratios. Mo isotope ratios in our study overlap with reference Mo isotope ratios within analytical error.