• Title/Summary/Keyword: Isotope

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Oxygen Isotope Study on the Wolf River Batholith, Wisconsin in U.S.A. (미국 위시컨신주의 올프리버 저반에 대한 산소동위원소 연구)

  • Sun-Joon Kim;Yuch-Ning Shieh
    • The Journal of the Petrological Society of Korea
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    • v.4 no.2
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    • pp.124-133
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    • 1995
  • Oxygen isotope compositions have been determined for the granitic and the related rocks from the Wolf River Ratholith, Wisconsin in U.S.A. Plutons which belong to the differentiation trend are almost identical in oxygen isotope fractionation, and plutons of undifferential sequences also show oxygen isotope compositions similar to each other, which show little isotope fractionations at high temperature range. In oxygen osotope composition, the country rocks (the Penokean plutonic rocks), which is higher by 1~2 permil than the batholith are improbable source of the batholith. However, the assimilation of parent magma of lower ${\delta}^{18}O$ values than the batholith with the Penokean plutonic rocks might have produced the batholith.

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Accurate Quantification of Saccharin Using Isotope Dilution Liquid Chromatography Mass Spectrometry (ID-LC/MS)

  • Lee, Yun-Jung;Kim, Byung-Joo;Kim, Jeong-Kwon;Ahn, Seong-Hee
    • Mass Spectrometry Letters
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    • v.2 no.2
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    • pp.37-40
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    • 2011
  • Saccharin is a commonly used artificial sweetener in foodstuffs. However, for its carcinogenic dispute, it has been regulated by government bodies. In this study, isotope dilution mass spectrometry (ID-MS) was introduced for the accurate quantification of saccharin. To employ ID-LC/MS, we obtained its isotope analogue, $^{13}C_1$-sodium saccharin, by customized synthesis. Samples were spiked with $^{13}C_1$-sodium saccharin and analyzed with LC/MS in negative mode. Chromatographic conditions were optimized for the adequate chromatographic retention and separation of saccharin with a $C_{18}$ column. MS was operated with electrospray ionization by the selected ion monitoring (SIM) mode of $[M-H]^-$ for saccharin (m/z 182) and $[M-Na]^-$ for its isotope analogue (m/z 183). To validate the ID-LC/MS method for accurate measurement, we prepared a batch of a candidate material by sortifying quasi-tea-drinks with saccharin and analyzed samples gravimetrically fortified in various levels of concentration. The repeatability and reproducibility of this method was tested by analyzing the reference material. Result show that ID-LC/MS is a reliable method for the quantitative analysis of saccharin.

Sensitivity studies on a novel nuclear forensics methodology for source reactor-type discrimination of separated weapons grade plutonium

  • Kitcher, Evans D.;Osborn, Jeremy M.;Chirayath, Sunil S.
    • Nuclear Engineering and Technology
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    • v.51 no.5
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    • pp.1355-1364
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    • 2019
  • A recently published nuclear forensics methodology for source discrimination of separated weapons-grade plutonium utilizes intra-element isotope ratios and a maximum likelihood formulation to identify the most likely source reactor-type, fuel burnup and time since irradiation of unknown material. Sensitivity studies performed here on the effects of random measurement error and the uncertainty in intra-element isotope ratio values show that different intra-element isotope ratios have disproportionate contributions to the determination of the reactor parameters. The methodology is robust to individual errors in measured intra-element isotope ratio values and even more so for uniform systematic errors due to competing effects on the predictions from the selected intra-element isotope ratios suite. For a unique sample-model pair, simulation uncertainties of up to 28% are acceptable without impeding successful source-reactor discrimination. However, for a generic sample with multiple plausible sources within the reactor library, uncertainties of 7% or less may be required. The results confirm the critical role of accurate reactor core physics, fuel burnup simulations and experimental measurements in the proposed methodology where increased simulation uncertainty is found to significantly affect the capability to discriminate between the reactors in the library.

Experimental validation of a nuclear forensics methodology for source reactor-type discrimination of chemically separated plutonium

  • Osborn, Jeremy M.;Glennon, Kevin J.;Kitcher, Evans D.;Burns, Jonathan D.;Folden, Charles M. III;Chirayath, Sunil S.
    • Nuclear Engineering and Technology
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    • v.51 no.2
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    • pp.384-393
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    • 2019
  • An experimental validation of a nuclear forensics methodology for the source reactor-type discrimination of separated weapons-useable plutonium is presented. The methodology uses measured values of intra-element isotope ratios of plutonium and fission product contaminants. MCNP radiation transport codes were used for various reactor core modeling and fuel burnup simulations. A reactor-dependent library of intra-element isotope ratio values as a function of burnup and time since irradiation was created from the simulation results. The experimental validation of the methodology was achieved by performing two low-burnup experimental irradiations, resulting in distinct fuel samples containing sub-milligram quantities of weapons-useable plutonium. The irradiated samples were subjected to gamma and mass spectrometry to measure several intra-element isotope ratios. For each reactor in the library, a maximum likelihood calculation was utilized to compare the measured and simulated intra-element isotope ratio values, producing a likelihood value which is proportional to the probability of observing the measured ratio values, given a particular reactor in the library. The measured intra-element isotope ratio values of both irradiated samples and its comparison with the simulation predictions using maximum likelihood analyses are presented. The analyses validate the nuclear forensics methodology developed.

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.

Feasibility Study of Isotope Ratio Analysis of Individual Uranium-Plutonium Mixed Oxide Particles with SIMS and ICP-MS

  • Esaka, Fumitaka;Magara, Masaaki;Suzuki, Daisuke;Miyamoto, Yutaka;Lee, Chi-Gyu;Kimura, Takaumi
    • Mass Spectrometry Letters
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    • v.2 no.4
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    • pp.80-83
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    • 2011
  • Isotope ratio analysis of nuclear materials in individual particles is of great importance for nuclear safeguards. Although secondary ion mass spectrometry (SIMS) and thermal ionization mass spectrometry (TIMS) are utilized for the analysis of individual uranium particles, few studies were conducted for the analysis of individual uranium-plutonium mixed oxide particles. In this study, we applied SIMS and inductively coupled plasma mass spectrometry (ICP-MS) to the isotope ratio analysis of individual U-Pu mixed oxide particles. In the analysis of individual U-Pu particles prepared from mixed solution of uranium and plutonium standard reference materials, accurate $^{235}U/^{238}U$, $^{240}Pu/^{239}Pu$ and $^{242}Pu/^{239}Pu$ isotope ratios were obtained with both methods. However, accurate analysis of $^{241}Pu/^{239}Pu$ isotope ratio was impossible, due to the interference of the $^{241}Am$ peak to the $^{241}Pu$ peak. In addition, it was indicated that the interference of the $^{238}UH$ peak to the $^{239}Pu$ peak has a possibility to prevent accurate analysis of plutonium isotope ratios. These problems would be avoided by a combination of ICP-MS and chemical separation of uranium, plutonium and americium in individual U-Pu particles.

Ginseng authenticity testing by measuring carbon, nitrogen, and sulfur stable isotope compositions that differ based on cultivation land and organic fertilizer type

  • Chung, Ill-Min;Lee, Taek-Jun;Oh, Yong-Taek;Ghimire, Bimal Kumar;Jang, In-Bae;Kim, Seung-Hyun
    • Journal of Ginseng Research
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    • v.41 no.2
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    • pp.195-200
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    • 2017
  • Background: The natural ratios of carbon (C), nitrogen (N), and sulfur (S) stable isotopes can be varied in some specific living organisms owing to various isotopic fractionation processes in nature. Therefore, the analysis of C, N, and S stable isotope ratios in ginseng can provide a feasible method for determining ginseng authenticity depending on the cultivation land and type of fertilizer. Methods: C, N, and S stable isotope composition in 6-yr-old ginseng roots (Jagyeongjong variety) was measured by isotope ratio mass spectrometry. Results: The type of cultivation land and organic fertilizers affected the C, N, and S stable isotope ratio in ginseng (p < 0.05). The ${\delta}^{15}N_{AIR}$ and ${\delta}^{34}S_{VCDT}$ values in ginseng roots more significantly discriminated the cultivation land and type of organic fertilizers in ginseng cultivation than the ${\delta}^{13}C_{VPDB}$ value. The combination of ${\delta}^{13}C_{VPDB}$, ${\delta}^{15}N_{AIR}$, or ${\delta}^{34}S_{VCDT}$ in ginseng, except the combination ${\delta}^{13}C_{VPDB}-^{34}S_{VCDT}$, showed a better discrimination depending on soil type or fertilizer type. Conclusion: This case study provides preliminary results about the variation of C, N, and S isotope composition in ginseng according to the cultivation soil type and organic fertilizer type. Hence, our findings are potentially applicable to evaluate ginseng authenticity depending on cultivation conditions.

Development of analytical method for the isotope purity of pure D2 gas using high-precision magnetic sector mass spectrometer

  • Chang, Jinwoo;Lee, Jin Bok;Kim, Jin Seog;Lee, Jin-Hong;Hong, Kiryong
    • Analytical Science and Technology
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    • v.35 no.5
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    • pp.205-211
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    • 2022
  • Deuterium (D) is an isotope with one more neutron number than hydrogen (H). Heavy elements rarely change their chemical properties with little effect even if the number of neutrons increases, but low-mass elements change their vibration energy, diffusion rate, and reaction rate because the effect cannot be ignored, which is called an isotope effect. Recently, in the semiconductor and display industries, there is a trend to replace hydrogen gas (H2) with deuterium gas (D2) in order to improve process stability and product quality by using the isotope effect. In addition, as the demand for D2 in industries increases, domestic gas producers are making efforts to produce and supply D2 on their own. In the case of high purity D2, most of them are produced by electrolysis of heavy water (D2O), and among D2, hydrogen deuteride (HD) molecules are present as isotope impurities. Therefore, in order to maximize the isotope effect of hydrogen in the electronic industry, HD, which is an isotope impurity of D2 used in the process, should be small amount. To this end, purity analysis of D2 for industrial processing is essential. In this study, HD quantitative analysis of D2 for high purity D2 purity analysis was established and hydrogen isotope RM (Reference material) was developed. Since hydrogen isotopes are difficult to analyze with general gas analysis instrument, they were analyzed using a high-precision mass spectrometer (Gas/MS, Finnigan MAT271). High purity HD gas was injected into Gas/MS, sensitivity was determined by a signal according to pressure, and HD concentrations in two bottles of D2 were quantified using the corresponding sensitivity. The amount fraction of HD in each D2 was (4518 ± 275) μmol/mol, (2282 ± 144) μmol/mol. D2, which quantifies HD amount using the developed quantitative analysis method, will be manufactured with hydrogen isotope RM and distributed for quality management and maintenance of electronic industries and gas producers in the future.

Chemical Compositions and Lead Isotope Ratios of Some Glass Beads from Seokga-tap, Gyeongju

  • Kang, Hyung-Tae;Yun, Eun-Young
    • Conservation and Restoration of Cultural Heritage
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    • v.1 no.1
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    • pp.3-8
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    • 2012
  • Chemical compositions and lead isotope ratios for four glass bead samples of Seokga-tap were analyzed and the results were organized. Among 4 glass beads found in the Seokga-tap, 3 pieces were lead glass. Manufacturing method was to firstly grind pebbles finely and mix lead ore to be melt at $740{\sim}760^{\circ}C$. The mixed ratio of silica and lead was 3:7. Moreover, The evaluation on the lead isotope ratio indicated that two lead glass pieces used lead ore from northern Korea. One piece has the direction of southern Korea lead ore, but it requires a further review. One glass bead of Seokga-tap was brown and it was potash lead glass ($K_2O-PbO-SiO_2$) System. The mixed ratio was approximately 50:10:40 for silica, natural saltpeter, and lead, respectively. Lead isotope ratio data fell within the lead ore from northern China. Therefore, it was concluded that potash lead glass found in the Seokga-tap was produced in northern area of China at the end of $10^{th}$ century and transferred to the Seokga-tap.

Errors in Isotope Dilution Caused by Matrix-induced Mass Bias Effect in Quadrupole Inductively Coupled Plasma-Mass Spectrometry

  • Pak, Yong-Nam
    • Bulletin of the Korean Chemical Society
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    • v.35 no.12
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    • pp.3482-3488
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    • 2014
  • Matrix-induced mass bias and its effect on the accuracy of isotope ratio measurements have been examined for a quadrupole-based inductively coupled plasma-mass spectrometer (Q ICP-MS). Matrix-induced mass bias effect was directly proportional to % mass difference, and its magnitude varied for element and nebulizer flow rate. For a given element and conditions in a day, the effect was consistent. The isotope ratio of Cd106/Cd114 under $200{\mu}g\;g^{-1}$ U matrix deviated from the natural value significantly by 3.5%. When Cd 111 and Cd114 were used for the quantification of Cd with isotope dilution (ID) method, the average of differences between the calculated and measured concentrations was -0.034% for samples without matrix ($0.076{\mu}g\;g^{-1}$ to $0.21{\mu}g\;g^{-1}$ for the period of 6 months). However, the error was as large as 1.5% for samples with $200{\mu}g\;g^{-1}$ U. The error in ID caused by matrix could be larger when larger mass difference isotopes are used.