• Title/Summary/Keyword: Isotope ratios

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Attenuation of Background Molecular Ions and Determination of Isotope Ratios by Inductively Coupled Plasma Mass Spectrometry at Cool Plasma Condition

  • 박창준
    • Bulletin of the Korean Chemical Society
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    • 제18권7호
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    • pp.706-710
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    • 1997
  • Isotope ratios of K, Ca, Cr and Fe are measured at cool plasma condition generated using high carrier flow rate and relatively low RF power of 900 W. Background molecular ions are suppressed to below 100 counts which give isobaric interference to the analytes. The background ions show different attenuation characteristics at increased carrier flow rate and hence for each element different carrier flow rate should be used to measure isotope ratios without isobaric interference. Isotope ratios are measured at both scan and peak-hopping modes and compared with certified or accepted ratios. The measured isotope ratios show some mass discrimination against low mass due to low ion energy induced from a copper shield to eliminate capacitive coupling of plasma with load coil.

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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    • 제4권4호
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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

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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    • 제51권5호
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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.

Carbon Stable Isotope Ratios of Phytoplankton and Benthic Diatoms in Lake Katanuma with Reference to Those of Other Lakes

  • Kikuchi, Eisuke;Takagi, Shigeto;Shikano, Shuichi;Hideyuki, Doi
    • 생태와환경
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    • 제38권spc호
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    • pp.8-11
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    • 2005
  • Carbon stable isotope ratios of producers varied in lake ecosystems. In tile present study, we tried to estimate the seasonal variations of carbon isotope ratios of phytoplankton and benthic diatoms in a strongly acidic lake ecosystem. Lake Katanuma is a volcanic, strongly acidic lake (average pH of 2.2), located in Miyagi, Japan. Only two algal species dominate in Lake Katanuma; Pinnularia acidojaponica as a benthic diatom, and Chlamydomonas acidophila as a green alga. Carbon isotope values of P. acidojaponica varied seasonally, while those of particulate organic matter, which were mainly composed of C. acidophila remained fairly stable. The differences suggested that $CO_2$ gas was more frequently limited for P. acidojaponica than C. acidophila, since high density patches of benthic diatoms were sometimes observed on the lake sediment. Generally, carbon concentration mechanisms (CCMs)of microalgae can fix bicarbonate in lakes, and affect the carbon isotope values of microalgae. While, in Lake Katanuma, CCMs of the microalgae may scarcely function because of high $CO_2$ gas concentration and low pH. This is the reason for low seasonal amplitude of carbon isotope values of phytoplankton relative to those in other lakes.

The Origin and Biogeochemistry of Organic Matter in Surface Sediments of Lake Shihwa and Lake Hwaong

  • Won, Eun-Ji;Cho, Hyen-Goo;Shin, Kyung-Hoon
    • Ocean Science Journal
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    • 제42권4호
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    • pp.223-230
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    • 2007
  • To understand the origin and biogeochemistry of the organic matter in surface sediments of Lake Shihwa and Lake Hwaong, organic nitrogen, inorganic nitrogen, labile organic carbon, and residual organic carbon contents as well as stable isotope ratios for carbon and nitrogen were determined by KOBr-KOH treatment. Ratios of organic carbon to organic nitrogen $(C_{org}/N_{org})$ (mean = 24) were much higher than ratios of organic carbon to total nitrogen $(C_{org}/N_{tot})$ (mean= 12), indicating the presence of significant amounts of inorganic nitrogen in the surface sediments of both lakes. Stable isotope ratios for organic nitrogen were, on average, $5.2\%_{\circ}$ heavier than ratios of inorganic nitrogen in Lake Shihwa, but those same ratios were comparable in Lake Hwaong. This might be due to differences in the origin or the degree of degradation of sedimentary organic matter between the two lakes. In addition, stable isotope ratios for labile organic carbon were, on average, $1.4\%_{\circ}$ heavier than those for residual organic carbon, reflecting the preferential oxidation of $^{13}C$-enriched organic matter. The present study demonstrates that KOBr-KOH treatment of sedimentary organic matter can provide valuable information for understanding the origin and degradation state of organic matter in marine and brackish sediments. This also suggests that the ratio of $(C_{org}/N_{org})$ and stable isotope ratios for organic nitrogen can be used as indexes of the degree of degradation of organic matter.

Determination of Li by Isotope Dilution Inductively Coupled Plasma Mass Spectrometry

  • Park, Chang J.;Chung, Bag S.
    • 분석과학
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    • 제8권4호
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    • pp.427-434
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    • 1995
  • Inductively coupled plasma mass spectrometry combined with the isotope dilution method is used for the determination of lithium. The isotope dilution method is based on the addition of a known amount of enriched isotope (spike) to a sample. The analyte concentration is obtained by measuring the altered isotope ratio. The spike solution is calibrated through so called reverse isotope dilution with a primary standard. The spike calibration is an important step to minimize error in the determined concentration. It has been found essential to add spike to a sample and the primary standard so that the two isotope ratios should be as dose as possible. Since lithium is neither corrosive nor toxic, lithium is used as a chemical tracer in the nuclear power plants to measure feedwater flow rate. 99.9% $^7Li$ was injected into a feedwater line of an experimental system and sample were taken downstream to be spiked with 95% $^6Li$ for the isotope dilution measurements. Effects of uncertainties in the spike enrichment and isotope ratio measurement error at various spike-to-sample ratios are presented together with the flow rate measurement results in comparison with a vortex flow meter.

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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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    • 제51권2호
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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.

탄소 및 질소 안정동위원소 비를 이용한 영산강하구역 유기물 기원 추정 연구 (Determination of the Origin of Particulate Organic Matter at the Estuary of Youngsan River using Stable Isotope Ratios (${\delta}^{13}C$, ${\delta}^{15}N$))

  • 이연정;정병관;신용식;김성환;신경훈
    • 생태와환경
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    • 제46권2호
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    • pp.175-184
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    • 2013
  • 본 연구는 영산강하구역 입자물질 유입원의 시 공간적인 변화를 추정해 보고자 몽탄대교에서 영산강 하구둑에 이르는 영산강하구역 세 정점에서 연 6회에 걸쳐 수 층 부유 물질의 탄소 및 질소 안정동위원소 비를 비교하였다. 모든 정점에서 8월에 강우를 통한 외부기원 유기물의 유입이 증가하였으며, 이 때 암모니아성 질소 및 규산염의 유입 역시 함께 증가하였다. 탄소 안정동위원소 비 측정 결과 11월과 8월에 정점 별 유기물의 기원이 크게 차이 났으며, 안정동위원소 비 값을 이용하여 주요 유입원 추정이 가능하였다. 11월에 모든 정점에서 질소 안정동위원소 비가 무거운 값을 보였고, 인산염의 농도가 가장 높게 나타났는데 이는 축산폐수 및 농경지를 통한 유입이 영향을 준 것으로 판단된다. 또한 다른 정점에 비해 영산강 하구둑에서 모든 조사 기간 동안 비교적 높은 질소 안정동위원소 비를 보였으며, 이를 통해 축산폐수 및 농경지를 통한 유기물 유입이 다른 정점에 비해 높을 것으로 추정된다. 본 연구 결과를 통해 안정동위원소 비 분석은 입자성유기물의 기원을 추정하는데 유용한 방법임을 확인할 수 있었다.

경복궁 청기와에 사용된 납유의 화학조성과 납동위원소 특성연구 (Study on the Chemical Composition and Lead Isotope Ratios of Lead Glaze Used on Blue Tiles from Gyeoungbokgung Palace)

  • 김소진;김영도
    • 자원환경지질
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    • 제57권3호
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    • pp.343-352
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    • 2024
  • 경복궁 전각 청기와에 사용된 납유의 발색 원리와 용융제로 사용된 납의 산지를 확인하기 위해 성분 분석과 납동위원소비 분석을 실시했다. 청기와 31점을 녹색, 청색, 황색으로 구분하여 표면에 시유된 납유의 성분을 분석한 결과 Pb, Si, Cu가 주성분으로, Fe, Ca, Mg, Al 등이 미량으로 검출되었다. 청색 납유에서는 Cu의 함량이 높았으며 황색 또는 갈색의 납유에서는 Cu는 검출되지 않았고 Fe의 함량이 높게 나타났다. 따라서 납유의 제작에 용융제로 납을, 발색제로 산화동을 사용했음을 알 수 있었다. 또한 경복궁 청기와에 사용된 납유의 납동위원소비는 한반도 납동위원소비 분포도에서 충청도와 전라도를 포함하는 zone 3 영역에 도시되었으며, 납유의 용융제는 이들 지역에서 산출되는 방연석 등을 사용했을 것으로 추정된다. 삼국과 통일신라시대 녹유의 납동위원소비는 대부분 한반도를 벗어나 위치하여 납의 산지가 변화되었음을 알 수 있었다. 특히 녹유 전돌의 납동위원소비를 통해 주변국과의 교류를 추정할 수 있었으며 동일 사찰에서 출토된 녹유 전돌의 납동위원소비가 서로 달라 다른 시기 또는 다른 공방에서 제작된 것으로 판단할 수 있었다.

Accurate determination of minor isotope ratios in individual plutonium-uranium mixed particles by thermal ionization mass spectrometry

  • Lee, Chi-Gyu;Park, Jinkyu;Lim, Sang Ho
    • Nuclear Engineering and Technology
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    • 제50권1호
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    • pp.140-144
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    • 2018
  • Isotopic analyses of plutonium and low-enriched uranium mixtures with particle sizes of $0.6-3.3{\mu}m$ were performed using thermal ionization mass spectrometry with a continuous heating method to verify its effectiveness for the accurate analysis of minor isotopes without sample pretreatment. The mixed particles used in this study were prepared from a mixed solution of plutonium (SRM 947) and uranium (U010, $^{235}U$ 1% enriched) reference materials. The isotope ratios for plutonium in the individual mixed particles, including $^{238}Pu/^{239}Pu$, $^{241}Pu/^{239}Pu$ as well as $^{240}Pu/^{239}Pu$, and $^{242}Pu/^{239}Pu$, were in good agreement with the certified values despite the isobaric interference of $^{238}U$ and $^{241}Am$. The isotope ratios for uranium in the mixed particles also agreed well with the certified values within the range of error. However, the isotope ratios for minor isotopes, such as $^{234}U$ and $^{236}U$, in the particles with diameters of less than approximately $1.8{\mu}m$ could not be measured because numbers of $^{234}U$ and $^{236}U$ atoms in analyzed particles are too low. These results indicate that thermal ionization mass spectrometry with a continuous heating method is applicable for the analysis of trace amounts of plutonium isotopes, including $^{238}Pu$ and $^{241}Pu$, despite the presence of the respective isobars $^{238}U$ and $^{241}Am$ in the microsamples.