• 제목/요약/키워드: isotope-ratio mass spectrometry

검색결과 42건 처리시간 0.024초

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

  • 임성아;한은미;채정석;윤주용
    • Journal of Radiation Protection and Research
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    • 제35권3호
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    • pp.117-123
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    • 2010
  • Pu 동위원소는 기원에 따라 각기 다른 $^{240}Pu/^{239}Pu$ 동위원소비를 나타내는 특성이 있다. 질량분석법은 극미량 장반감기핵종 분석에 매우 유용한 방법으로서 검출기 특성상 낮은 검출한계를 갖고 있으며, 소량의 시료를 이용하여 짧은 시간에 측정을 할 수 있다는 장점을 갖고 있으므로 Pu을 비롯한 장반감기 핵종 분석에 유용하다. 다중검출기유도결합플라즈마질량분석기(Multicollector ICP-MS)는 다중검출시스템을 이용하여 분석하고자 하는 여러 핵종의 동시분석이 가능하며, 특별히 본 연구에서는 극미량 핵종의 검출이 가능한 multiple ion counter (MIC)를 사용하여 Pu 동위원소 분석에 적용하였다. 본 연구방법의 검출한계(detection limit)는 최적화된 조건에서 $^{239}Pu$$^{240}Pu$ 각각 $0.10\;fg\;ml^{-1}$ ($0.24\;{\mu}Bq\;ml^{-1}$), $0.12\;fg\;ml^{-1}$ ($0.97\;{\mu}Bq\;ml^{-1}$)이었으며, 240Pu 기준으로 약 200 cps 정도의 매우 낮은 농도수준에서 1%이하의 $^{240}Pu/^{239}Pu$ 동위원소비 계측편차를 나타내었다. 본 연구방법은 표준용액 및 다양한 매트릭스의 표준물질 분석에 적용함으로써 검증 확인하였다.

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.

Looking through the Mass-to-Charge Ratio: Past, Present and Future Perspectives

  • Shin, Seung Koo
    • Mass Spectrometry Letters
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    • 제12권4호
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    • pp.126-130
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    • 2021
  • The mass spectrometry (MS) provides the mass-to-charge ratios of atoms, molecules, stable/metastable complexes, and their fragments. I have taken a long journey with MS to address outstanding issues and problems by experiments and theory and gain insights into underlying principles in chemistry. By looking through the mass-to-charge ratio, I have studied thermochemical problems in silicon chemistry, the infrared multiphoton dissociation spectroscopy of organometallic intermediates, unimolecular dissociations of halotoluene radical cations, and the kinetics of association/dissociation of alkali halide triple ions with Lewis bases. Various MS platforms have been used to characterize non-covalent interactions between porphyrins and fullerenes and those between the group IIB ions and trioctylchalcogenides, and to examine the binding of the group IA, IIA and porphyrin ions to G-quadruplex DNA. Recently, I have focused on mass-balanced H/D isotope dipeptide tags for MS-based quantitative proteomics, a simple chemical modification method for MS-based lipase assay, and the kinetics and dynamics of energy-variable collision-induced dissociation of chemically modified peptides. Now, I see an important role of MS in global issues in the post-COVID era, as the society demands high standards for indoor air quality to contain the airborne-pathogen transmission as well as in-situ monitoring and tracking of carbon emissions to reduce global warming.

Validation and Applications of Gas Chromatography-Combustion/isotope Ratio Mass Spectrometric Method to Control Misuse of Androgens in Human

  • Lee, Kang-Mi;Kim, Ho-Jun;Jeong, Eun-Sook;Yoo, Hye-Hyun;Kwon, Oh-Seung;Jin, Chang-Bae;Kim, Dong-Hyun;Lee, Jae-Ick
    • Mass Spectrometry Letters
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    • 제2권2호
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    • pp.33-36
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    • 2011
  • The misuse of anabolic androgenic steroids is of particular concern in sports and society. Thus, it is of great importance to discriminate endogenous steroids such as testosterone or testosterone prohormones from their chemically identical synthetic copies. In this study, gas chromatography-combustion/isotope ratio mass spectrometric (GC-C/IRMS) method has been developed and validated for discriminating the origin of anabolic androgenic steroids. The method involves the solid-phase extraction, enzymatic hydrolysis with ${\beta}$-glucuronidase, HPLC-fractionation for the cleanup and analysis by GC-C/IRMS. The difference(${\Delta}^{13}C$) of urinary ${\delta}^{13}C$ values between synthetic analogues and endogenous reference compounds (ERC) by GC-C/IRMS was used to elucidate the origin of steroids, and intra- and inter-day precision, specificity and isotope fractionation were evaluated. The present GC-C/IRMS method combined with HPLC cleanup was accurate and reproducible enough to be successfully applied to the test of urine sample from suspected anabolic steroid abusers.

Methodological Study on Measurement of Hydrogen Abundance in Hydrogen Isotopes System by Low Resolution Mass Spectrometry

  • Lia, Jin-Ying;Shib, Lei;Hub, Shi-Lin
    • Mass Spectrometry Letters
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    • 제2권1호
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    • pp.1-7
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    • 2011
  • China's rapid economic growth has resulted in significant environmental side effects. Therefore, China has been interested in reducing her dependence on foreign oil and gas by developing technologies needed for hydrogen, in addition to her increasing energy mix of nuclear and renewable energy form, such as solar and wind power. There are three isotopes of hydrogen, i.e. protium (P or H), deuterium (D), and tritium (T). Both deuterium and tritium are important materials in nuclear fuel cycle industry. Tritium is one of the critical radioactive nuclides. Planning for and implementing contamination control as a part of normal operation and maintenance activities is an important function in any hydrogen facility, especially tritium facility. The development of hydrogen isotopes analysis is the key issues in this area. Mass spectrometry (MS) with medium (about 600) and high resolution (> 1,400) is commercially available; however, the routine analysis of hydrogen isotopes is done with low-resolution MS (< 200) in China. This paper summarizes the progress of MS measurement technology for hydrogen isotope abundance in China, focusing on our lab's research program and technical status. An analyzing method has been introduced for accurate measurement of tritium abundance in the H.D.T system by low resolution MAT-253 MS. The quotient of compression ratio coefficient is determined by building up equipment for laboratory-scale preparation of secondary standard gases and by considering the difference in sensitivity between hydrogen isotopes. The results show that the measured value is reproducible within the relative error range of 0.8% for gas samples of different tritium abundance.

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

  • 이신우;박재선;박현우;황종연;김금희;정현미;최종우
    • 환경분석과 독성보건
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    • 제21권4호
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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.

GC/MS에 의한 한국인의 모발중 Methamphetamine검출 (Determination of methamphetamine in the hair of Korean abuser by CG/MS)

  • 유영찬;정희선;최화경
    • 약학회지
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    • 제37권4호
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    • pp.356-361
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    • 1993
  • A sensitive method for the determination of methamphetamine(MA) and amphetamine(AM) in hair was developed by gas chromatography/mass spectrometry using stable isotope-labeled internal standards, amphetamine-d$_{5}$ and methamphetamine-d$_{5}$. Hair sample was washed with MeOH, incubated with MeOH(I% HCI) overnight at $37^{\circ}C$ while stirring and extracted using solid phase extraction column on a vacuum manifold. The extract obtained was pentafluoropropionated, and applied to GC/MS. The calibration curves of MA and AM were linear from 2.5 to 250 ng (r>0.99 for both). The limit of detection was 0.1 ng/mg in hair and cut-off level was set at 0.25 ng/mg for both. Hair samples of 27 MA abusers showed positive results in the range 0.7 to 106.8 ng/mg. AM, its metabolite, was detected in 20 out of 27 samples. The ratio of MA versus AM was 4.6~38.3 in specimens. Hair analysis for methamphetamine by GC/MS is an effective method for identifying long-term drug abusers.

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Complete Genome and Calcium Carbonate Precipitation of Alkaliphilic Bacillus sp. AK13 for Self-Healing Concrete

  • Jung, Yoonhee;Kim, Wonjae;Kim, Wook;Park, Woojun
    • Journal of Microbiology and Biotechnology
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    • 제30권3호
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    • pp.404-416
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    • 2020
  • Bacteria that are resistant to high temperatures and alkaline environments are essential for the biological repair of damaged concrete. Alkaliphilic and halotolerant Bacillus sp. AK13 was isolated from the rhizosphere of Miscanthus sacchariflorus. Unlike other tested Bacillus species, the AK13 strain grows at pH 13 and withstands 11% (w/v) NaCl. Growth of the AK13 strain at elevated pH without urea promoted calcium carbonate (CaCO3) formation. Irregular vaterite-like CaCO3 minerals that were tightly attached to cells were observed using field-emission scanning electron microscopy. Energy-dispersive X-ray spectrometry, confocal laser scanning microscopy, and X-ray diffraction analyses confirmed the presence of CaCO3 around the cell. Isotope ration mass spectrometry analysis confirmed that the majority of CO32- ions in the CaCO3 were produced by cellular respiration rather than being derived from atmospheric carbon dioxide. The minerals produced from calcium acetate-added growth medium formed smaller crystals than those formed in calcium lactate-added medium. Strain AK13 appears to heal cracks on mortar specimens when applied as a pelletized spore powder. Alkaliphilic Bacillus sp. AK13 is a promising candidate for self-healing agents in concrete.

Application of Stable Isotope Ratio Analysis for Origin Authentication of Pork

  • Kim, Kyong Su;Kim, Jae Sung;Hwang, In Min;Jeong, In Seon;Khan, Naeem;Lee, Sun Im;Jeon, Dong Bok;Song, Yang Hoon;Kim, Kwan Suk
    • 한국축산식품학회지
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    • 제33권1호
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    • pp.39-44
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    • 2013
  • Origin authenticity of the animals used as food has always been a major concern to consumers around the world. In the past twenty years, a stable isotope ratio has been used for origin authentication. In this study, pork samples, both local and imported, were collected from the major markets from all around South Korea and analyzed for stable isotope ratios of nitrogen (${\delta}^{15}N$‰) and carbon (${\delta}^{13}C$‰), using Isotope Ratio Mass Spectrometry (IR-MS). A total of 599 samples with 335 Korean and 264 imported from 13 countries within America and Europe were investigated in accordance to the standard established methods for isotope ratio analysis. The results showed a significant variation related to the origin of the samples, explaining the difference in the feeding styles of the pork in each country. The stable isotope ratio values of carbon (${\delta}^{13}C$‰) were found in the decreasing order of: America ($-15.55{\pm}1.01$‰)>Korea ($-19.62{\pm}0.89$‰)>Europe ($-24.79{\pm}1.35$‰). Canada was having ${\delta}^{13}C$ ratio of $-22.87{\pm}0.92$‰, which is very low in the region of America and very close to Europe (-23.78 to -27.17‰). For nitrogen ${\delta}^{15}N$‰ the order was: America ($4.92{\pm}0.71$‰)>Europe ($4.54{\pm}0.66$‰)>Korea ($3.69{\pm}0.54$‰), with a slight variation among countries in each region studied. From the results it was concluded that the stable isotope ratio of the pork samples from different countries provide enough information about the origin and is therefore a potential tool which can be employed for origin authentication.

레이저 이온화 이온트랩 질량분석법을 이용한 금속 및 세라믹 시료의 원소분석에 관한 연구 (Study on elemental analysis of metal and ceramic samples by using laser ablation ion trap mass spectrometry(LAITMS))

  • 송규석;박현국;차형기;이상천
    • 분석과학
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    • 제15권1호
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    • pp.7-14
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    • 2002
  • 본 연구에서는 레이저 애블레이션 이온 트랩 질량분석법을 이용하여 금속 및 세라믹 시료들에 대한 원소분석을 수행하였고, 이때 이온화 장치로는 XeCI 엑시머 레이저를 사용하였고 검출장치로서 이온트랩 질량 분석기를 사용하였다. 시료는 트랩의 바깥에 장착하여 시료의 교환이 매우 쉽도록 하였고 고체시료의 분석에 있어서 매우 효과적임을 밝혔다. 헬륨기체의 압력이나 이온저장시간, 초기질량제한 RF 전압 등에 대한 기초 실험을 통하여 실험의 최적 조건을 구하였고 (헬륨 기체압력 $1{\times}10^{-4}$ Torr 이온 저장시간 100 ms 초기 질량 제한전압 $1150V_{p-p}$), 이 결과를 토대로 금속시료(구리, 몰리브데늄)와 세라믹 시료(알루미나 세라믹, 지르코니아 세라믹) 들에 대한 원소분석을 수행하였다.