• Title/Summary/Keyword: EPMA analysis

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A way Analyzing Oxide Layer on an Irradiated CANDU-PHWR Pressure Tube Using an EPMA and X-ray Image Mapping

  • Jung, Yang Hong;Kim, Hee Moon
    • Corrosion Science and Technology
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    • v.20 no.3
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    • pp.118-128
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    • 2021
  • The oxide layer in samples taken from an irradiated Zr-2.5Nb pressure tube from a CANDU-PHWR reactor was analyzed using electron probe microanalysis (EPMA). The examined tube had been exposed to temperatures ranging from 264 to 306 ℃ and a neutron fluence of 8.9 × 1021 n/cm2 (E > 1 MeV) for the maximum 10 effective full-power years in a nuclear power plant. Measuring oxide layer thickness generally employs optical microscopy. However, in this study, analysis of the oxide layer from the irradiated pressure tube components was undertaken through X-ray image mapping obtained using EPMA. The oxide layer characteristics were analyzed by X-ray image mapping with 256 × 256 pixels using EPMA. In addition, the slope of the oxide layer was measured for each location. A particular advantage of this study was that backscattered electrons and X-ray image mapping were obtained at a magnification of 9,000 when 20 kV volts and 30 uA of current were applied to radiation-shielded EPMA. The results of this study should usefully contribute to the study of the oxide layer properties of various types of metallic materials irradiated by high radiation in nuclear power plants.

EPMA Analysis of Inter-reaction Layer in Irradiated U3Si-Al Fuels (EPMA를 이용한 U3Si/Al 조사 핵연료의 반응층 분석)

  • Jung, Yang-Hong;Yoo, Byung-Ok;Kim, Hee-Moon;Park, Jong-Man;Kim, Myung-Han
    • Analytical Science and Technology
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    • v.17 no.4
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    • pp.355-362
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    • 2004
  • Fission products and Inter reaction layer of $U_3Si-Al$ dispersion fuel, irradiated in HANARO research reactor with 121 kW/m of maximum liner power and 63 at% of average burn-up, was characterization by EPMA (Electron Probe Micro Analyzer). The fuel punching system developed by Irradiated Materials Examination Facility (IMEF) has used to make these samples for the EPMA. With this system a very small and thin specimen which is 1.57 mm in diameter and 2 mm in thickness respectively has been fabricated to protect the EPMA operator from high radioactive fuel and to mini-mize the equivalent dose rate less than 150 mSv/h. EPMA was performed to observe layers of sectional, Inter-reaction and oxide with specimens of cutting and polished. Stoichiometry in the Inter-reaction layer with $16{\mu}m$ of thickness was $U_{2.84}$ Si $Al_{14}$ with calibration of $UO_2$ and $U_{3.24}$ Si $Al_{14.1}$ with calibration of standard specimen. metallic precipitates in this layer were not observed using fission products examination.

The analysis of the deposit on inner steam generator by EPMA (EPMA를 이용한 증기발생기 내부 침적물 분석)

  • 유병옥;정양홍;김도식;백승제;김기하;주용선;박남홍;이종헌
    • Proceedings of the Korean Radioactive Waste Society Conference
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    • 2004.06a
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    • pp.230-231
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    • 2004
  • 경수로형 원자로의 증기 발생기 내부에 방사화 된 침적물을 smear paper로 시료를 채취한여 핵종 분석 및 화학조성을 분석하였다. 상용발전소의 증기 발생기 외부에서 발견된 고 준위 방사성물질의 화학 조성 분석은 극미세 성분분석기(EPMA)를 이용하였다. 본 시험에 사용한 EPMA(Electron Probe Micro Analyzer, SX-50R, CAMECA, Paris, France)는 고 방사능을 띤 조사 핵연료 및 재료 시험을 수행할 수 있도록 기기의 시편 stage 주위를 납과 텅스텐으로 차폐하여 시편의 방사능 세기가 $3.7{\times}10^{10}$ Bq까지 시험 가능한 기기이다.(중략)

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Single Particle Analysis of Aerosols collected at Seoul, CheongJu, and ChunCheon, Using Low-Z Electron Probe X-ray Microanalysis (Low-Z Electron Probe X-ray Microanalysis를 이용한 서울, 청주, 춘천의 입자상 물질 분석)

  • ;;;;R. Van Grieken
    • Proceedings of the Korea Air Pollution Research Association Conference
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    • 2001.11a
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    • pp.307-308
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    • 2001
  • 본 연구는 서울, 청주, 춘천 세 개 도시 대기에서의 입자상 물질에 대한 분석을 Electron Probe X-ray Microanalysis(EPMA)를 이용한 단일 입자 분석법으로 행하였다. 단일 입자 분석법은 개개 입자의 형상과 크기 그리고 화학 조성에 대한 정보를 동시에 제공하기 때문에 개개 입자의 생성, 이동, 반응 그리고 환경에의 영향에 대한 자세한 정보를 얻을 수 있다. 또한 최근에 개발된 ultrathin window를 장착한 EPMA 분석법(Low-Z EPMA)은 종래의 통상적인 EPMA 방법으로는 분석하기 어려웠던 탄소, 질소, 산소 등의 원소를 정량적으로 분석할 수 있다. 따라서 도시 대기의 중요 구성 입자상 물질인 황산염, 질산염, 암모늄염, 유기 입자 등도 포함하여 도시 대기 입자 분석에 유용하게 활용된다. (중략)

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Characterization of Individual Atmospheric Particles, Collected in Susan, Korea, Using Low-Z Electron Probe X-ray Microanalysis (Low-Z Electron Probe X-ray Microanalysis 분석법을 이용한 해안인근 지역의 대기입자 분석)

  • 김혜경;노철언
    • Journal of Korean Society for Atmospheric Environment
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    • v.19 no.5
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    • pp.503-513
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    • 2003
  • A single particle analytical technique, called low-Z electron probe X-ray microanalysis (low-Z EPMA) was applied to characterize atmospheric particles collected in Busan, Korea, over a daytime period in Dec. 2001. The ability to quantitatively analyze the low-Z elements, such as C, N, and 0, in microscopic volume enables the low-Z EPMA to specify the chemical composition of individual atmospheric particle. Various types of atmospheric particles such as organics, carbon-rich, aluminosilicates, silicon oxide, calcium carbonate, iron oxide, sodium chloride, sodium nitrate, ammonium sulfate, and titanium oxide were identified. In the sample collected in Busan, sodium nitrate particles produced as a result of the reaction between sea salt and nitrogen oxides in the atmosphere were most abundantly encountered both in the coarse and fine fractions. On the contrary, original sea salt particles were rarely observed. The fact that most of the carbonaceous particles were distributed in the fine fraction implies that their origin is anthropogenic.

Analysis of Heterogeneous $CaCO_{3}-CaSO_{4}$ Single Particle using Ultra-thin Window EPMA (Ultra-thin Window EPMA를 이용한 $CaCO_{3}-CaSO_{4}$ 혼성의 단일 입자 분석)

  • ;;R. Van Grieken
    • Proceedings of the Korea Air Pollution Research Association Conference
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    • 2000.11a
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    • pp.87-90
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    • 2000
  • 대기 중에 존재하는 화합물의 반응을 연구하는 것은 대기 오염 화합물의 이동이나 소멸, 환경에의 영향을 파악하기 위하여 긴요하다. 특히 입자상 물질과 기체상 화합물과의 반응을 명확히 이해하는 것은 대기 오염물질의 거동을 파악하는데 매우 중요하다. 입자상 물질을 분석하는 방법 중에 EPMA(Electron Probe X-ray Microanalysis)를 이용한 단일 입자 분석법(Single Particle Analysis)은 개개 입자의 형상과 크기 그리고 화학 조성에 대한 정보를 동시에 제공하기 때문에 개개 입자의 생성, 이동, 반응성, 소멸 그리고 환경에의 영향에 대한 자세한 정보를 얻을 수 있다. (중략)

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Single Particle Analysis of Atmospheric Aerosol Particles Collected in Seoul, 2001, Using Low-Z Particle Electron Probe X-ray Microanalysis (Low-Z Particle Electron Probe X-ray Microanalysis를 이용한 2001년 서울시 대기 중 입자상 물질 분석)

  • Koo Hee Joon;Kim HyeKyeong;Ro Chul-Un
    • Journal of Korean Society for Atmospheric Environment
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    • v.20 no.6
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    • pp.823-832
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    • 2004
  • Atmospheric aerosol particles collected in Seoul on four single days, each in every seasons of 2001, were characterized and classified on the basis of their chemical species using low-Z particle electron probe X-ray microanalysis (low-Z particle EPMA). Low-Z particle EPMA technique can analyze both the size and the chemical species of individual aerosol particles of micrometer size and provide detailed information on the size distribution of each chemical species. The major chemical species observed in Seoul aerosol were aluminosilicate, silicon dioxide, calcium carbonate, organic, carbon-rich, marine originated, and ammonium sulfate particles, etc. The soil originated species, such as aluminosilicate, silicon dioxide, and calcium carbonate were the most popular in the coarse fraction, meanwhile, carbonaceous and ammonium sulfate were the dominant species found in the fine fraction. Marine originated species such as sodium nitrate was frequently encountered, up to 30% of the analyzed aerosol particles.

Correction for Na Migration Effects in Silicate Glasses During Electron Microprobe Analysis (전자현미분석에서 발생하는 규산염 유리 시료의 Na 이동 효과 보정)

  • Hwayoung, Kim;Changkun, Park
    • Korean Journal of Mineralogy and Petrology
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    • v.35 no.4
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    • pp.457-467
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    • 2022
  • Electron bombardment to silicate glass during electron probe microanalysis (EPMA) causes outward migration of Na from the excitation volume and subsequent decrease in the measured X-ray count rates of Na. To acquire precise Na2O content of silicate glass, one should use proper analytical technique to avoid or minimize Na migration effect or should correct for decreases in the measured Na X-ray counts. In this study, we analyzed 8 silicate glass standard samples using automated Time Dependent Intensity (TDI) correction method of Probe for EPMA software that can calculate zero-time intercept by extrapolating X-ray count changes over analysis time. We evaluated an accuracy of TDI correction for Na measurements of silicate glasses with EPMA at 15 kV acceleration voltage and 20 nA probe current electron beam, which is commonly utilized analytical condition for geological samples. Results show that Na loss can be avoided with 20 ㎛-sized large beam (<0.1 nA/㎛2), thus silicate glasses can be analyzed without TDI correction. When the beam size is smaller than 10 ㎛, Na loss results in large relative errors up to -55% of Na2O values without correction. By applying TDI corrections, we can acquire Na2O values close to the reference values with relative errors of ~ ±10%. Use of weighted linear-fit can reduce relative errors down to ±6%. Thus, quantitative analysis of silicate glasses with EPMA is required for TDI correction for alkali elements such as Na and K.