• Title/Summary/Keyword: 원소분석

Search Result 2,520, Processing Time 0.027 seconds

Determination of Uranium Isotopes in Spent Nuclear Fuels by Isotope Dilution Mass Spectrometry (동위원소희석 질량분석법을 이용한 사용후핵연료 중 우라늄 동위원소 정량)

  • Kim, Jung Suk;Jeon, Young Shin;Son, Se Chul;Park, Soon Dal;Kim, Jong Goo;Kim, Won Ho
    • Analytical Science and Technology
    • /
    • v.16 no.6
    • /
    • pp.450-457
    • /
    • 2003
  • The determination of uranium and its isotopes in spent nuclear fuels by isotope dilution mass spectrometry (IDMS) has been studied. The spent fuel samples were dissolved in 8 M $HNO_3$ or its mixture with 14 M $HNO_3-0.05M$ HF. The dissolved solutions were filterred on membrane filter with $1.2{\mu}m$ pore size. The uraniums in the spiked and unspiked sample solutions were quantitatively adsorbed by anion exchange resin, AG 1X8 and eluted with 0.1 M HCl. The contents of uranium and its isotopes ($^{234}U$, $^{235}U$, $^{236}U$$^{238}U$) in the spent fuel samples were determined by isotope dilution mass spectrometric method using $^{233}U$ as spike. The spike reference solution was standarized by reverse isotope dilution mass spectrometry (R-IDMS) using natural and depleted uranium. The results from IDMS were in average relative difference of 0.34% when compared with those by the potentiometric titration method.

Development of a Noble Gas Isotope Dilution Mass Spectrometric System Combined with a Cryogenic Cold Trap (초저온 냉각 트랩을 결합한 비활성기체 동위원소 희석 질량분석 시스템의 제작)

  • HONG, BONGJAE;SHIN, DONGYOUB;PARK, KEYHONG;HAHM, DOSHIK
    • The Sea:JOURNAL OF THE KOREAN SOCIETY OF OCEANOGRAPHY
    • /
    • v.27 no.3
    • /
    • pp.144-157
    • /
    • 2022
  • Noble gases, which are chemically inert and behave conservatively in marine environments, have been used as tracers of physical processes such as air-sea gas exchange, mixing of water masses, and distribution of glacial meltwater in the ocean. For precise measurements of Ne, Ar, and Kr, we developed a mass spectrometric system consisting of a quadrupole mass spectrometer (QMS), a high vacuum preparation line, an activated charcoal cryogenic trap (ACC), and a set of isotope standard gases. The high vacuum line consists of three sections: (1) a sample extraction section that extracts the dissolved gases in the sample and mixes them with the standard gases, (2) a gas preparation section that removes reactive gases using getters and separates the noble gases according to their evaporation points with the ACC, and (3) a gas analysis section that measures concentrations of each noble gas. The ACC attached to the gas preparation section markedly lowered the partial pressures of Ar and CO2 in the QMS, which resulted in a reduced uncertainty of Ne isotope analysis. The isotope standard gases were prepared by mixing 22Ne, 36Ar, and 86Kr. The amounts of each element in the mixed standard gases were determined by the reverse isotope dilution method with repeated measurements of the atmosphere. The analytical system achieved precisions for Ne, Ar, and Kr concentrations of 0.7%, 0.7%, and 0.4%, respectively. The accuracies confirmed by the analyses of air-equilibrated water were 0.5%, 1.0%, and 1.7% for Ne, Ar, and Kr, respectively.

Determination of trace actinide (Am, Pu, Th, U) using alpha spectrometry and neutron activation analysis (알파분광법과 중성자방사화분석법에 의한 극미량의 악티늄계원소 (Am, Pu, Th, U)분석연구)

  • Yoon, Yoon Yeol;Lee, Kil Yong;Cho, Soo Young;Kim, Yongjai;Lee, Myong Ho
    • Analytical Science and Technology
    • /
    • v.17 no.4
    • /
    • pp.302-307
    • /
    • 2004
  • Determination of actinides in the environmental sample requires separation of each element. This procedure is tedious and time consuming. And also, the detection limits of some nuclides using alpha spectrometry are rather higher. To overcome the lower detection limit and complicated separation procedure, a simple analytical technique for the determination of actinide isotopes in the environmental samples was developed and applied to IAEA and NIST reference sediment samples. For the separation of actinides from matrix, anion exchange resin and TRU-spec extraction chromatography resin were used and chemical yields were obtained using natural uranium, thorium, $^{242}Pu$ and $^{243}Am$ tracers. For overcoming the higher detection limits of U and Th in alpha spectrometry, neutron activation analysis was applied. Using combined method, the detection limit was increased about 10 times. The activity values of each isotope were consistent with the reference values reported by IAEA and NIST.

Analysis of Charred-Woods Excavated from the Daewoongjeon Hall of Youngguksa Temple (영국사 대웅전 출토 탄화목의 재질 분석)

  • Son, Byung Hwa;Park, Won-Kyu
    • Journal of the Korean Wood Science and Technology
    • /
    • v.35 no.1
    • /
    • pp.36-43
    • /
    • 2007
  • Elemental analysis, SEM-EDX, X-ray diffraction (XRD) and IR analysis were adopted to examine the quality of charred woods excavated from the underground of the Daewoongjeon Hall of Youngguksa Temple, Youngdong-gun, Chungbuk, Korea. A large amount of calcium was detected in SEM-EDX analysis. The analyses of chemical elements suggested that completely charred wood was carbonized at about $500^{\circ}C$. The XRD results indicated the destruction of cellulose crystalline region. The IR analysis exhibited that thermal degradation of wood component was different depending upon the carbonization temperature. It can be suggested from the results that PEG with different molecular weights should be used for the conservation of excavated charred woods.

Quality Assurance of the Analysis of Airborne Trace Metals (대기중 미량금속분석의 정도 관리)

  • 장미숙;임종명;이현석;이진홍
    • Proceedings of the Korea Air Pollution Research Association Conference
    • /
    • 2002.04a
    • /
    • pp.143-144
    • /
    • 2002
  • 본 연구는 대전 1,2 공단지역을 대상으로 22개의 금속원소를 ICP-MS를 이용하여 분석한 후, 이 농도 자료에 바탕하여 사용여지별 원소의 정밀도를 평가하고, 2 단계 선별과정을 통한 분석 농도의 대표성을 평가하고자 한다. (중략)

  • PDF

Analysis of rifle and pistol primer gunshot residue using SEM-EDX (SEM-EDX에 의한 소총과 권총의 뇌관화약잔사 분석)

  • Jeon, Chung-Hyun;Park, Sung-Woo
    • Analytical Science and Technology
    • /
    • v.23 no.3
    • /
    • pp.322-329
    • /
    • 2010
  • Primer gunsot residues (GSR) obtained from K1A and K2 rifles, and K5 pistol were analysed with scanning electron microscopy/energy dispersive X-ray spectrometry (SEM-EDX) as basic data in firearm accidents. Ammunition of 5.56 mm is employed for K1A and K2 rifles and 9.0 mm for a K5 pistol. The analyses of morphology, size, particle number, elemental ratio were performed for primer GSR prepared after shooting 3 times. The detected content was Ba>Pb>Sb in most GSR particles but Sb>Pb>Ba or Pb>Sb>Ba in some particles. In the statistical result of composition ratio of elements, the particles with more Sb than Ba were detected in most primer GSR from a K5 pistol, 3~8 times more than K1A and K2 rifles. This results can be employed to discriminate gun type between rifles and pistols. Furthermore, the size and the number of particles can be applied to access the type of guns.

고에너지 중이온 TOF-ERDA를 이용한 박막분석

  • Hong, Wan;Woo, Hyung-Joo;Kim, Young-Seok;Kim, Gi-Dong;Kim, Jun-Gon;Choi, Han-Woo
    • Proceedings of the Korean Vacuum Society Conference
    • /
    • 1999.07a
    • /
    • pp.77-77
    • /
    • 1999
  • 박막시료의 분석에는 RBS, XPS, SIMS, AES 등이 주로 이용되고 있으며, 특히 RBS는 비교체가 필요없고 정량성이 좋다는 장점 때문에 중요하다. 그러나 RBS는 원리적으로 경원소에 대한 감도가 낮아 기판원소보다 무거운 질량을 갖는 원소의 분석에만 이용되는 것이 보통이다. 이러한 단점을 보완하기 위해 본 연구에서는 수년전부터 RBS와 비슷한 원리를 갖고 같은 장비를 이용하여 수행이 가능한 경원소 분석법인 TOF-ERDA(Time of Flight Elastic Recoil detection)을 개발하여 실용화 하였다. 본 연구실에서 보유하고 있는 미국 NEC사의 5SDH 가속기는 최대 가속전압이 1.7MV로 Cl5+ 이온을 사용하는 경우 10 MeV가 최대 가속에너지가 된다. 이런 정도의 에너지 범위에서는 TOF spectrometer의 시간분해능이 아주 높을 필요가 없고 비교적 작은 가속기로도 분석이 가능하며, 수소의 검출효율이 우수하다는 점 등 많은 장점이 있다. 그러나 한편으로는 분석가능한 깊이가 수천 $\AA$ 정도로 제한되고 질량 분해능도 수십 MeV 내지 100MeV 이상의 고에너지 이온빔을 이용하는 경우에 비해 떨어진다는 단점이 있다. 또한 묵운 원소의 분석이 불가능하기 때문에 경원소의 분석에 국한하여 적용하고 무거운 원소에 대해서는 RBS를 병용하게 된다. 본 연구에서는 일본 이화학연구소의 선형가속기인 RILAC으로부터 얻은 40MeV Ar 이온 및 138 MeV Xe 이온을 이용하여 TOF-ERDA 시스템을 제작하였다. 그러기 위해서 고에너지 이온의 비행시간을 측정하는 목적으로 높은 시간 분해능을 갖는 시간 검출기를 설계, 제작하였다. 또한 표적함 밑에는 회전원판이 있어 시간검출기 및 에너지 검출기가 중앙의 시료홀더를 중심으로 회전이 가능하도록 되었다. 회전은 표적함 밖에서 원격조정 가능하다. 이렇게 함으로써 검출각을 임의로 바꾸면서 측정이 가능하도록 하였다. 제작된 분석시스템의 성능을 확인하기 위해 YBaCuO 초전도 박막을 측정하였으며 그 결과를 그림에 나타낸다. 저 에너지 ERDA에서는 나타나기 힘든 Ba, Y, Cu 등의 무거운 원소의 피크들이 분명히 나타남을 확인할 수 있다.

  • PDF