• Title/Summary/Keyword: Oxidized Sample

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Modification of conventional X-ray diffractometer for the measurement of phase distribution in a narrow region

  • Park, Yang-Soon;Han, Sun-Ho;Kim, Jong-Goo;Jee, Kwang-Yong;Kim, Won-Ho
    • Analytical Science and Technology
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    • v.19 no.5
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    • pp.407-414
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    • 2006
  • An X-ray diffractometer for spatially resolved X-ray diffraction measurements was developed to identify phase in the narrow (micron-scaled) region of high burn-up fuels and some nuclear materials. The micro-XRD was composed of an X-ray microbeam alignment system and a sample micro translation system instead of a normal slit and a fixed sample stage in a commercial XRD. The X-ray microbeam alignment system was fabricated with a microbeam concentrator having two Ni deposited mirrors, a vertical positioner, and a tilt table for the generation of a concentrated microbeam. The sample micro translation system was made with a sample holder and a horizontal translator, allowing movement of a specimen at $5{\mu}m$ steps. The angular intensity profile of the microbeam generated through a concentrator was symmetric and not distorted. The size of the microbeam was $4,000{\times}20{\mu}m$ and the spatial resolution of the beam was $47{\mu}m$ at the sample position. When the diffraction peaks were measured for a $UO_2$ pellet specimen by this system, the reproducibility ($2{\Theta}={\pm}0.01^{\circ}$) of the peaks was as good as a conventional X-ray diffractometer. For the cross section of oxidized titanium metal, not only $TiO_2$ in an outer layer but also TiO near an oxide-metal interface was observed.

High Temperature Stability of Sintered Bulk CrN (CrN 소결체의 고온 안정성)

  • Choi, J.H.;Lee, D.B.
    • Journal of the Korean institute of surface engineering
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    • v.40 no.1
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    • pp.39-43
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    • 2007
  • The pure CrN powders oxidized to $Cr_2O_3$ noticeably above $850^{\circ}C$ in air. When these powders were sintered into bulk samples at $1500^{\circ}C$ under 40 atm of $N_2$ pressure, the CrN phase partly changed into the $Cr_2N$ phase, owing to the partial loss of nitrogen from CrN. When the bulk sample was heated at $1000-1200^{\circ}C$ for 100 hr under vacuum, the CrN phase also progressively changed into $Cr_2N$. At the same time, a relatively thin $Cr_2O_3$ layer formed on the bulk sample due to the reaction of chromium with residual oxygen in vacuum.

Sonochemical Reaction Mechanism of a Polycyclic Aromatic Sulfur Hydrocarbon in Aqueous Phase

  • Kim, Il-Kyu;Jung, Oh-Jin
    • Bulletin of the Korean Chemical Society
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    • v.23 no.7
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    • pp.990-994
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    • 2002
  • Hydroxybenzothiophenes, dihydroxy-benzothiophenes, and benzothiophenedione were identified as inter-mediates of benzothiophene (BT) exposed to ultrasonic irradiation. It is proposed that benzothiophene is oxidized by OH radical to sequentially for m hydroxybenzothiophenes, dihydroxybenzothiophenes, and benzothiophenedione. Benzothiophene is decomposed rapidly following pseudo-first-order kinetics in a first-order manner by ultrasonic irradiation in aqueous solution. The toxicity of sonochemically treated solutions was checked by E. coli and a less inhibition in bacterial respiration was observed from the 120-min treated benzothiophene sample than from the untreated benzothiophene sample. Also evolution of carbon dioxide and sulfite was observed during ultrasonic reaction. A pathway for ultrasonic decomposition of benzothiophene in aqueous solution is proposed.

A STUDY ON OXIDATION TREATMENT OF URANIUM METAL CHIP UNDER CONTROLLING ATMOSPHERE FOR SAFE STORAGE

  • Kim, Chang-Kyu;Ji, Chul-Goo;Bae, Sang-Oh;Woo, Yoon-Myeoung;Kim, Jong-Goo;Ha, Yeong-Keong
    • Nuclear Engineering and Technology
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    • v.43 no.4
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    • pp.391-398
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    • 2011
  • The U metal chips generated in developing nuclear fuel and a gamma radioisotope shield have been stored under immersion of water in KAERI. When the water of the storing vessels vaporizes or drains due to unexpected leaking, the U metal chips are able to open to air. A new oxidation treatment process was raised for a long time safe storage with concepts of drying under vacuum, evaporating the containing water and organic material with elevating temperature, and oxidizing the uranium metal chips at an appropriate high temperature under conditions of controlling the feeding rate of oxygen gas. In order to optimize the oxidation process the uranium metal chips were completely dried at higher temperature than $300^{\circ}C$ and tested for oxidation at various temperatures, which are $300^{\circ}C$, $400^{\circ}C$, and $500^{\circ}C$. When the oxidation temperature was $400^{\circ}C$, the oxidized sample for 7 hours showed a temperature rise of $60^{\circ}C$ in the self-ignition test. But the oxidized sample for 14 hours revealed a slight temperature rise of $7^{\circ}C$ representing a stable behavior in the self-ignition test. When the temperature was $500^{\circ}C$, the shorter oxidation for 7 hours appeared to be enough because the self-ignition test represented no temperature rise. By using several chemical analyses such as carbon content determination, X-ray deflection (XRD), Infrared spectra (IR) and Thermal gravimetric analysis (TGA) on the oxidation treated samples, the results of self-ignition test of new oxidation treatment process for U metal chip were interpreted and supported.

Effect of Plasma Oxidation lime on TMR Devices of CoFe/AlO/CoFe/NiFe Structure (절연막층의 플라즈마 산화시간에 따른 CoFe/AlO/CoFe/NiFe 구조의 터널자기저항 효과 연구)

  • 이영민;송오성
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.15 no.4
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    • pp.373-379
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    • 2002
  • We investigated the evolution of magnetoresistance and magnetic property of tunneling magnetoresistive(TMR) device with microstructure and plasma oxidation time. TMR devices have potential applications for non volatile MRAM and high density HDD reading head. We prepared the tunnel magnetoresistance(TMR) devices of Ta($50{\AA}$)/NiFe($50{\AA}$)/IrMn($150{\AA}$)/CoFe($50{\AA}$)/Al($13{\AA}$)-O/CoFe($40{\AA}$)/FiFe($400{\AA}$)/Ta(($50{\AA}$) structure which have $100{\times}100\mu\textrm{m}^2$ junction area on $2.5{\times}2.5\textrm{cm}^2$ Si/$SiO_2$(($1000{\AA}$) substrates by an inductively coupled plasma(ICP) magnetron sputter. We fabricated the insulating layer using an ICP plasma oxidation method by with various oxidation time from 30 sec to 360 sec, and measured resistances and magnetoresistance(MR) ratios of TMR devices. We found that the oxidized sample for oxidation time of 80 sec showed the highest MR radio of 30.31 %, while the calculated value regarding inhomogeneous current effect indicated 25.18 %. We used transmission electron microscope(TEM) to investigate microstructural evolution of insulating layer. Comparing the cross-sectional TEM images at oxidation time of 150 sec and 360 sec, we found that the thickness and thickness variation of 360 sec-oxidized insulating layer became 30% and 40% larger than those of 150 sec-oxidized layer, repectively. Therefore, our results imply that increase of thickness variation with oxidation time may be one of the major treasons of the MR decrease.

Development of Immunological Methods for Analysis of 5' -deoxy-5' -methylthioadenosine

  • Lee, Sung-Ho;Cho, Young-Dong
    • BMB Reports
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    • v.30 no.6
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    • pp.403-409
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    • 1997
  • Studies were undertaken to develop a competitive radioimmunoassay (RIA) and indirect antigen capture enzyme-linked immunosorbent assay (ELISA) for the determination of 5'-deoxy-5'-methylthioadenosine (MTA), which is formed from decarboxylated S-adenosylmethionine by spermidine and spermine synthase. Specific antiserum against MTA was raised in rabbits by immunization with MTA-BSA which was prepared by coupling BSA to oxidized MTA with periodate. Since MTA is oxidized easily to the sulfoxide, the sulfhydryl reagent, DTT. was added to the immunogen. For RIA, immunocomplexes were separated from free MTA by using ammonium sulfate precipitation. The antiserum showed almost no cross-reactivity with a variety of other nucleotides and riboses. But, the level of cross-reactivity of 5'-isobutylthioadenosine (SIBA) was high. These results showed the importance of hydrophobicity adjacent to the 5'-OH for determining antigenicity. The lower limit of detection by this assay was 100 fmol of MTA per tube. Using this assay. MTA levels were more easily and precisely determined in biological samples when compared with HPLC analysis. The RIA procedure is less time consuming. More than 24 analyses can be carried out in 2 h and required only a very small amount of sample ($20{\mu}l$ serum). In ELISA, biotin conjugated MTA-BSA was used as the labelled MTA. The sensitivity limit of this assay was lower than 100 pmol.

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Effects of Surface Roughness on the Thermal Emissivity of IG-11 Graphite for Nuclear Reactor (IG-11 원자로용 흑연의 열방사 특성에 미치는 표면 거칠기의 영향)

  • Roh, Jae-Seung;Seo, Seung-Kuk;Kim, Suk Hwan;Chi, Se-Hwan;Kim, Eung-Seon;Kim, Hye Sung
    • Korean Journal of Metals and Materials
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    • v.49 no.7
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    • pp.557-564
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    • 2011
  • This paper reports the relationship between the surface roughness and thermal emissivity of graphite (IG-11) in nuclear reactors. The roughness was controlled by changing the oxidization time, resulting in 0, 6, and 11% losses of mass. The levels of roughness were 0.40, 0.72 and 1.09${\mu}m$ for the weight loss of 0, 6 and 11%, respectively. The binders and graphite fillers were found to have sequentially oxidized with a higher thermal emission for the highly oxidized sample, but with a lower emission when measured at a higher temperature. Our study suggests a method for predicting the thermal emission rate of graphite in a nuclear reactor based on roughness measurement.

Surface Analysis Study on ZIRLO Cladding Hulls Oxidized at Low Temperatures (저온 산화된 ZIRLO 피복관의 표면분석 연구)

  • Jeon, Min Ku;Choi, Yong Taek;Lee, Chang Hwa;Kang, Kweon Ho;Park, Geun Il
    • Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
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    • v.12 no.3
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    • pp.235-243
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    • 2014
  • Surface oxidation behavior of ZIRLO (ZIRconium Low Oxidation) hulls was investigated using an X-ray photoelectron spectroscopy (XPS) technique. The effects of oxidation time (10-336 h at $500^{\circ}C$) and temperature ($400-700^{\circ}C$ for 10 h) were studied. Deconvolution results of the hulls oxidized at $500^{\circ}C$ revealed that a $ZrO_2$ phase appeared after 24 h (11.86%), and an increase in the $ZrO_2$ ratio was observed when the hulls were oxidized for 336 h (17.93%). On the other hand, the ZrO phase which employed 5.68% in the 10 h oxidized sample disappeared when the oxidation time increased to 24 h. The XPS results also showed that an increase in the oxidation temperature resulted in an increase in the ratio of ZrO, which increased from 0 to 5.68, 8.31, and 9.16% when the oxidation temperature increased from 400 to 500, 600, and $700^{\circ}C$, respectively. $ZrO_2$ phase was observed only in the sample that was oxidized at $700^{\circ}C$. The mechanism of ZrO formation was not conclusive, but it was suggested that a formation of hydroxide might have been accelerated at elevated temperatures leading to a formation of a $Zr(OH)_4$ phase. The relationship between the surface oxidation status of the hulls oxidized at $500^{\circ}C$ and their chlorination reaction feasibility was discussed, and it was suggested that the thickness of the oxide layer is an important parameter that determines the chlorination reaction feasibility.

Comparison of Oxidative Stability for the Thermally-oxidized Vegetable Oils using a DPPH Method (DPPH법에 의한 식용유지의 열산화 안정성 비교)

  • Lee, Jae-Min;Chang, Pahn-Shick;Lee, Jae-Hwan
    • Korean Journal of Food Science and Technology
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    • v.39 no.2
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    • pp.133-137
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    • 2007
  • The 2,2-diphenyl picrylhydrazyl (DPPH) method, which can be used to predict the oxidative stability of edible oils, was previously reported by our research group. Not only free radical scavenging antioxidants but also radicals from oxidized oils are capable of reacting with DPPH radicals, thereby reducing the absorbance of DPPH. In this study, the optimum sample size of edible oils for the DPPH method was determined, and the oxidation of the edible oils was monitored via DPPH, coupled with other conventional methods. The optimum sample size was determined as 1.5 g using soybean oil. Soybean, corn, virgin olive, and refined olive oils were thermally oxidized for 3 hr at $180^{\circ}C$ and analyzed via DPPH, conjugated dienoic acid (CDA) value, and p-anisidine value (p-AV) protocols. Soybean and corn oils were found to be more sensitive to thermal oxidation than virgin and refined olive oils, on the basis of the CDA value and p-AV measurements. The DPPH method can indicate the inherent radical scavenging activity of unoxidized samples, the time required for the depletion of antioxidants, and the rate of degradation of the antioxidants. The soybean and corn oils evidenced higher levels of free radical scavenging compounds, required more time for the consumption of inherent antioxidants, and also manifested steeper antioxidant degradation rates than olive oils, based on the results of DPPH analysis. The DPPH method, accompanied by other conventional methods, may prove useful in predicting the degree of oxidation of vegetable oils.

Enhancement of Antioxidation Effect of Platycodon grandiflorum with Vitamin C on the DLPC Liposomes (DLPC Liposome에 미치는 도라지 추출성분의 비타민 C 첨가에 의한 항산화력 상승효과)

  • 배송자;강보영;김미향
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.31 no.3
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    • pp.506-510
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    • 2002
  • The effect of antioxidant activity of Platycodon grandiflorum (PG) on the liposomal phospholipid membrane was investigated by spectrophotometry. Membrane oxidation causes damage to the membrane fluidity and permeability. It brings further destruction to the sustenance of biological homeostasis. In addition, it is related to several diseases, aging and carcinogenesis. The sample PG was extracted and fractionated to five different types; butanol (PGMB), ethylacetate (PGMEA), ethylether (PGMEE), hexane (PGMH) and methanol (PGMM). The oxidation indices of PGMEA and PGMEE fractions in oxidized dilinoleoylphosphatidylcholine (DLPC) liposomes had stronger antioxidant activities than that of ${\alpha}$-tocopherol and were similar to antioxidant activities compared with butylated hydroxy toluene (BHT), a well-known potent antioxidant, in oxidized DLPC liposomes. The oxidation indices of PGMM extract, PGMB and PGMH fractions exhibited weak antioxidant activity compared with ${\alpha}$-tocopherol in oxidized DLPC liposomes. The oxidation indiex of PGMEE fractions added with vitamin C showed even strong antioxidant activity in the oxidized DLPC liposomes. The oxidation activity of BHT with vitamin C also proved to be stronger than BHT without vitamin C. Therefore vitamin C evidently helps to improve the effect of antioxidant in DLPC liposomes. These results indicate that potentially bioactive substances in PGMEE fraction has a function as potent antioxidant against phospholipid membrane oxidation.