• Analytical Science and Technology
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• v.22 no.2
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• pp.186-190
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• 2009

The oxidation studies of a sulfur to a sulfate ion by various oxyhalide oxidants in organic (thiourea, methionine) and inorganic (sulfate, thiophosphate) compounds were carried out in an acidic solution. The optimized result of the oxidation reaction was obtained when a bromate compound (${BrO_3}^-$) as an oxidant and a 3 M $HNO_3$ solvent were used. The chemical yield for the oxidation of the organic and inorganic sulfur compounds to a sulfate ion was monitored as 80% for thiophosphate, 87% for methionine, and 100% for thiourea and sulfate within 5% RSD. The oxidations of thiourea required at least 1.6 equivalents of the bromate in an acidic solution. In the case of the oxidation of methionine and thiophosphate, the oxidation yields were above 80% if the bromate was used at 20 times higher than that of the substrates. The sulfate ion was quantitatively measured by using a GPC counting of $^{35}S$ followed by precipitates of $BaSO_4$. A quenching correction curve for the $^{35}S$ counting was obtained to use the difference via the precipitate weight result.

• Journal of the Korean Chemical Society
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• v.45 no.4
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• pp.298-303
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• 2001

The trace-level mercury in bio-materials has been determinated by the anodic stripping square wave voltammetry (ASSWV)-technique at glassy carbon electrode. Prior to the analysis, the bio-materials were digested with $HNO_3/H_2SO_4$ mixture and KMnO4 was added to complete an oxidation process of the mixture. The detection limit of the mercury varied greatly with deposition time, deposition potential, pH and stirring rate. When the deposition was carried out for 240 sec on 400 rpm stirring at -1.0 volts vs. Ag/AgCl, the detection limit was below 0.5 ppb ($2.5{\times}10^{-9}M$). The accumulated mercury was high in the kidney and liver, and low in the brain according to the determination of mercury accumulation for a white rat by this method.

• Journal of the Korean institute of surface engineering
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• v.45 no.5
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• pp.198-205
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• 2012

The corrosion properties of anodized films on aluminium 6070 alloy in a sulfuric acid have been studied. Comparison to evaluate the anodized A6070 and pure 6070 specimen, corrosion tests in $HNO_3$ vapor environment of the 20 wt.% were performed up to 72 hours. Characteristics of film formation and surface morphology were examined by optical microscopy, FE-SEM, and EDS. The oxide film anodized in the sulfuric acid solution contained 5 to 10 wt.% of sulfur. In the initial stages of corrosion, anodized specimens exhibited corrosion resistance than the pure specimen. However, the corrosion conditions in 24 hours, corrosion was far more anodized specimen than pure specimen. Therefore, anodized films contained sulfur, nitric acid vapor in the environment is thought to stimulate corrosion.

• Analytical Science and Technology
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• v.5 no.1
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• pp.143-152
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• 1992

Corrosion resistances in various acids and high temperature oxidation properties have been investigated for the Ni-base superalloy KM 1557. Corrosion tests were performed in $H_2SO_4$, HCl, $HNO_3$, $H_3PO_4$ and $CH_3COOH$. Oxidation tests were carried out in air for 20 and 110hrs at $900^{\circ}C$, $950^{\circ}C$ and $1050^{\circ}C$. Hot corrosion tests were done in salt bath of 75% $Na_2SO_4-25%$ NaCl at $900^{\circ}C$ for 20hrs. After the tests, the samples were observed by optical microscopy and analysed by EPMA and X-ray mapping in order to investigate the distribution of composition. It was shown that corrosion resistances in various acids and hot salt bath were proven to be excellent. It was suggested that the amounts of oxides were determined mainly by the depth of internal and intergranular $Al_2O_3$ oxide layers.

• Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
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• v.5 no.3
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• pp.179-188
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• 2007

In this work $^{14}C\;and\;^3H$ distribution characteristics of spent resins from nuclear power plants(NPPs), pressurized water reactors(PWRs), was investigated. It was found that the recovery percent of $^{14}C$ by the wet oxidation-acid stripping was $81%{\sim}100%$ for the added activity range of $^{14}C,\;0.72\;Bq{\sim}460\;Bq$, and it was not affected by the kinds of stripping acids, 3N-HCl, $3\;N-HNO_3\;and\;3\;N-H_2SO_4$. And the recovery percent of $^3H$ by distillation using the same apparatus was $81%{\sim}101%$ for the added activity range of $^3H,\;0.60\;Bq{\sim}435\;Bq$. Among the tested stripping acids, 3\;N-HCl, $3\;N-HNO_3\;and\;3\;N-H_2SO_4$, only the trapped $^3H$ solution by distillation in $3\;N-H_2SO_4$ was compatible with the 3H scintillator, Ultimagold XR. Neither of the $^{14}C\;and\;^3H$ trapping solutions from the spent ion exchange resin samples by the wet oxidation-3 $N-H_2SO_4$ stripping contained gamma nuclides. However, some gamma nuclides, $^{60}Co,\;^{134}Cs,\;^{137}Cs\;and\;^{54}Mn$, were found in the trapped $^3H$ solutions of the spent resins by the wet oxidation-3 N-HCl stripping. It was the same for the $^3H$ trapping solutions of the spent resins by Sample Oxidizer(PACKARD MODEL 307). Meanwhile only two nuclides, $^{134}Cs,\;and\;^{134}Cs$, were found in the $^{14}C$ trapping solutions of the spent resins by Sample Oxidizer(PACKARD MODEL 307). It was found that most of the $^{14}C$ in the spent resins existed as inorganic carbon form, more than about 70% of the total $^{14}C$ content. Among the analyzed 30 spent ion exchange resin samples, the average concentration of $^{14}C$ and $^3C$ for the high radioactive samples, 8 samples, was $19000\;Bq/g{\pm}41000\;Bq/g,\;670\;Bq/g{\pm}460\;Bq/g$ and that for the low radioactive samples, 22 samples, was $4.2\;Bq/g{\pm}4.3\;Bq/g,\;6.0\;Bq/g{\pm}5.3\;Bq/g$, respectively. And the average $^{14}C/^3H$ ratio for the high radioactive samples, was higher, 28, than that of low radioactive samples, 0.70. Some linear relationship trend was found between the activity concentrations of $^{14}C\;and\;^3H$.

• Applied Chemistry for Engineering
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• v.18 no.3
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• pp.291-295
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• 2007

The oxidation treatment of needle cokes with 70 wt% of nitric acid and sodium chlorate ($NaClO_3$) was attempted to achieve an electrochemically active material with a large capacitance. The structure of needle cokes was changed to graphite oxide after oxidation treatment of needle cokes with acidic solution having the composition ratio, $NaClO_3$/needle cokes, of 7.5, and the inter-layer distance of the oxidized needle cokes was extended to $6.9{\AA}$with increasing oxygen content. On the other hand, the electrochemical performance of oxidized needle cokes as a polarized electrode for an Electric Double Layer Capacitor (EDLC) was examined with an electrolyte of 1.2 M $TEABF_4$ (tetraethylammonium tetrafluoroborate) and $TEABF_4$ (triethylmethylammonium tetrafluoroborate) in acetonitrile. The capacitor cell using 1.2 M $TEABF_4$/acetonitrile has exhibited smaller electric resistance of $0.05{\Omega}$, and larger capacitance per weight and volume of 32.0 F/g and 25.5 F/mL at the two-electrode system in the potential range 0~2.5 V than that of the capacitor cell using $TEABF_4$. The observed electrochemical performance was discussed with the correlation between the inter-layer distance in graphite oxide structure and the anionic size of electrolyte.

• Polymer(Korea)
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• v.37 no.1
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• pp.61-65
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• 2013

In this work, the anodic oxidation of carbon fibers was carried out to enhance the mechanical interfacial properties of carbon fibers-reinforced epoxy matrix composites. The surface characteristics of the carbon fibers were studied by FTIR, X-ray photoelectron spectroscopy (XPS), and scanning electron microscopy (SEM). Also, the mechanical interfacial properties of the composites were studied with interlaminar shear strength (ILSS), critical stress intensity factor ($K_{IC}$), and critical strain energy release rate ($G_{IC}$). The anodic oxidation led to a significant change in the surface characteristics of the carbon fibers. The anodic oxidation of carbon fiber improved the mechanical interfacial properties, such as ILSS, $K_{IC}$, and $G_{IC}$ of the composites. The mechanical interfacial properties of the composites anodized at 20% sulfuric/nitric (3/1) were the highest values among the anodized carbon fibers. These results were attributed to the increase of the degree of adhesion at interfaces between the carbon fibers and the matrix resins in the composite systems.

• Journal of Korean Society of Environmental Engineers
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• v.33 no.2
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• pp.137-142
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• 2011

This study was conducted to establish the optimal electrolyte and bismuth concentrations using bismuth film electrode in laboratory and to confirm the possibilities of using this operational condition for heavy metals monitoring in field. In lab test, heavy metal measurement was not accurate more than 600 ppb when heavy metal (Pb, Cd, Zn) range 100~1,000 ppb was measured with bismuth 2,000 ppb. So, bismuth and heavy metal was reacted about 1:1 with ASV method. In electrolyte test, 0.1 M acetate buffer (pH 4.5), 0.1 M chloroacetate buffer (pH 2.0), 0.1 M HCl (pH 2.0), 0.1 M $HNO_3$ (pH 2.0) was tested. As a results, 0.1 M acetate buffer was most suitable in ASV measurement with bismuth film electrode. In field application, Pb, Cd and Zn was measured respectively 36~45 ppb, 84~91 ppb, 90~98 ppb when heavy metal (Pb, Cd, Zn) 100 ppb was spiked in field sample. These results were identified of matrix effect in field sample, So relationship between heavy metal measurement and matrix effects will be studied.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.28 no.2
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• pp.85-90
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• 2018

For the recovering rare earths in the spent nickel-metal hydride batteries, 10 M NaOH is added to the solution leached with sulfuric acid. The rare earth powders were precipitated at rate of 98 % at the condition of pH 2.0 or less. The recovered rare earth complex precipitate increased the leaching rate to nitric acid by heat treatment at $800^{\circ}C$ for 4 hours. Subsequently secondary precipitation was performed by adding oxalic acid to the solution in which the rare earth complex precipitate was dissolved. The re-precipitated rare earth powders were converted into oxide form through heat treatment at $800^{\circ}C$ for 4 hours with purity of 99.5 %.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2002.11a
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• pp.313-316
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• 2002

비철금속 습식 제련용 고효율 장수명의 양극을 개발하기 위해서 산소 과전압이 낮은 $MnO_{2}$를 촉매로 사용하여 반도체 산화물계의 산소선택성 전극을 제조하고 산화물 coating층의 미세구조와 전기화학적 특성을 분석하였다. PVDF : $MnO_{2}$의 함량비플 1 : 1 에서 1 : 40까지 정량적으로 변화시켰고， 용제의 점도에 지배적인 영향을 미치는 DMF의 함량을 각각의 고정된 PVDF : $MnO_{2}$의 함량비에서 변화시켜 용제를 제조하였으며 4% $HNO_{3}$ 용액에 세척된 Pb전극을 1.5 mm/sec 의 속도로 5회 dipping 하였다. PVDF : $MnO_{2}$ = 1 : 6인 경우 PVDF의 양이 증가하고 DMF의 양이 감소할수록 피막층이 두꺼워지고 PVDF : DMF = 4 : 96인 경우 pb 전극의 피막층이 얇기 때문에 박리현상이 일어났으며 이는 산화물 용제의 낮은 점도 때문인 것으로 판단된다. 또한 PVDF : DMF = 10 : 90의 경우는 5회 dipping 하여 약 $150{\mu}m$의 피막층을 형성하였다. PVDF : Mn02의 함량비가 1:1에서 1:6 까지는 DMF의 함량에 무관하게 전극 특성이 나타나지 않았지만 $MnO_{2}$의 양이 상대적으로 증가하면 cycle 이 증가하더라도 거의 일정한 전류 값을 갖고$MnO_2$와 PVDF의 비가 20:1 이상의 조성에서는 균일한 CV 특성을 나타냈다 이는 $MnO_{2}$가 효과적으로 촉매 작용을 한 것으로 판단되며 anodic polarization에 의한 산소 발생 과전압도 약 1.4V 정도로 감소되었다.