• Analytical Science and Technology
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• v.13 no.6
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• pp.751-758
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• 2000

A study was carried out on the dissolution of spent PWR fuels and performed on the fuels and the separation of iodide for the quantitative analysis using SIMFUEL which has chemical composition of a simulated spent PWR fuel (burn-up; 35,000 MWd/MTU and cooling time; 10 years). To dissolve the SIMFUEL effectively and to minimize the formation of volatile iodine through dissolution process, the optimum ratio of mixed acid ($HNO_3/HCl$ 80: 20 mol%) was established and ozone gas was purged. In the separation step of iodine with $CCl_4$, $NH_2OH{\cdot}HCl$ was used for reducing ${IO_3}^-$ to $I_2$.The optimum acidity of the dissolved solution and the added of $NH_2OH{\cdot}HCl$ were 2.5 M and more than $1.5{\times}10^{-3}mole$, respectively. The recovery of iodide by ion chromatography was $82.8{\pm}4.1%$ and the total yield was corrected by gamma spectrometery using $^{131}I$ as a tracer.

• KSBB Journal
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• v.24 no.3
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• pp.303-311
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• 2009

A scaling up study for the exopolysaccharide (EPS) production by submerged culture of Ganoderma lucidum was carried out in jar fermenter systems (2.6, 20 and 75 L) under bi-staged pH process. Profiles of dissolved oxygen (DO) and volumetric coefficient of oxygen transfer ($k_La$) as a function of operating variables (agitation speed and aeration rate) was investigated, and a correlation between $k_La$ and operating variables was analysed statistically. Under bi-staged pH process, no limitation of DO was observed at agitation speeds tested in the range of 200 and 600 rpm, and the highest EPS production was obtained at the level of DO of $40{\sim}80%$. From the regression analysis, the relation between $k_La$, gas velocity (Vs), stirrer speed (N) and impeller diameter (Di) could be expressed as : $$k_La=0.555{\times}Vs^{0.42}{\times}(N^3{\times}Di^2)^{0.33}\;(R^2=0.925,\;p<0.05)$$ It was found that under 2.6 L jar fermenter, the optimum agitation speed and aeration rate was 400 rpm and 1 vvm, respectively, obtaining the EPS production of 15.43 g/L. Under the submerged cultivation of G. lucidum in jar fermenters of $2.6{\sim}75\;L$, the similar EPS yields at each fermenter were achieved during scaling up based on $k_La$, and $k_La$ value for maximum EPS production was $85.4{\pm}26.70\;h^{-1}$.

• Journal of the Korean Chemical Society
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• v.36 no.2
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• pp.255-260
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• 1992

A procedure for spectrophotometric determination of traces of phosphorus(P) in high-purity trichlorosilane(TCS) is proposed using an adsorptive separation. $PCl_3$, which is a dominant P impurity within TCS, is first oxidized by oxygen to a stable form as $POCl_3$. $AlCl_3$ is selected as an adsorbent which forms a thermally stable complex with $POCl_3$ in TCS and can be well dissolved in aqueous ethanol solution. The proposed adsorptive separation method is free from the formation of silica gel and gas bubbles during the colorimetric analysis of TCS. The method reveals that the P concentration in a semiconductor-grade TCS is 5.32 ${\mi}g/l$ within the standard deviation of ${\pm}$ 17%. On the other hand, the P concentration of the purified TCS which is separated from the $AlCl_3$${\cdot}$$POCl_3$ complex is reduced to be less than 0.15 ${\mi}g/l$, showing the efficient applicability of $AlCl_3$ to the wet chemical analysis. The proposed method is also tested to verify the effectiveness of other well-known adsorbents.

• Journal of the Korean Chemical Society
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• v.40 no.12
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• pp.724-732
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• 1996

The organic precipitate flotation using Cu(II)-pyrrolidinedithiocarbamate complex as a coprecipitant was studied for the preconcentration and determination of trace Cd, Pb, Bi and Co in several water samples. Experimental conditions such as pH of solution, amounts of Cu(II) and ammonium pyrrolidinedithiocarbamate(APDC), stirring time, the type and amount of surfactant, etc. were optimized for the effective flotation of analytes. After 3.0 mL of 1,000 ${\mu}g/mL$ Cu(II) solution was added to 1.00 L water sample, the pH of the solution was adjusted to 2.5 with HNO3 solution. Trace amounts of analytes were coprecipitated by adding 2.0% APDC solution. And the precipitates were flotated onto the surface of solution with the aid of nitrogen gas and sodium lauryl sulfate. The floats were collected from mother liquor, and filtered through the micropore glass filter by suction. The precipitates were dissolved with 4 mL conc. HNO3, and then diluted to 25.00 mL with deionized water. The analytes were determined by graphite furnace atomic absorption spectrophotometry. This flotation technique was applied to the analysis of some water samples, and the 90 to 120% of recoveries were obtained from the spiked samples, this procedure could be concluded to be simple and applicable for the trace element analysis in various kinds of water.

• Analytical Science and Technology
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• v.22 no.6
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• pp.514-518
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• 2009

Coenzyme $Q_{10}$($CoQ_{10}$), a vitamin E-like substance, represents a components of the complex antioxidant system of the human organism. $CoQ_{10}$ levels in human plasma were determined by high performance liquid chromatography (HPLC) with UV detection. It was dissociated from lipoproteins by methanol and extracted into n-hexane with liquid-liquid extraction procedure, after centrifugation, the supernatant was dried under nitrogen gas stream. The residue was dissolved in the absolute ethanol. Determination of $CoQ_{10}$ was performed on a $C_{18}$ reversed-phase analytical column with ultraviolet detection at 275 nm and the mobile phase containing 15% (v/v) ethanol in methanol at a flow rate of 1.7 mL/min. The low limit of quantitation was 0.02 mg/L (S/N=10), the linearity between the concentration and peak height is from 0.1 to 2.0 mg/L. Twenty-four randomly selected plasma samples from apparently healthy, 27 to 44 year old individuals (males and females) were analyzed for total $CoQ_{10}$. The average level in these subjects was $0.62{\pm}0.13mg/L$ with the range of 0.41-0.98 mg/L. This method has a specific and a sufficient limit of quantitation (LOQ) for analysis of $CoQ_{10}$ in human plasma in both a clinical study and research at laboratories.

• Journal of Welding and Joining
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• v.30 no.1
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• pp.64-71
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• 2012

The characteristics of high heat input (342kJ/cm) EG (Electro Gas Arc) welded joint of EH36-TM steel has been investigated. The weld metal microstructure consisted of fine acicular ferrite (AF), a little volume of polygonal ferrite (PF) and grain boundary ferrite (GBF). Charpy impact test results of the weld metal and heat affected zone (HAZ) met the requirement of classification rule (Min. 34J at $-20^{\circ}C$). In order to evaluate the relationship between the impact toughness property and the grain size of HAZ, the austenite grain size of HAZ was measured. The prior austenite grain size in Fusion line (F.L+0.1 mm) was about $350{\mu}m$. The grain size in F.L+1.5 mm was measured to be less than $30{\mu}m$ and this region was identified as being included in FGHAZ(Fine Grain HAZ). It is seen that as the austenite grain size decreases, the size of GBF, FSP (Ferrite Side Plate) become smaller and the impact toughness of HAZ increases. Therefore, the CGHAZ was considered to be area up to 1.3mm away from the fusion line. Results of TEM replica analysis for a welded joint implied that very small size ($0.8\sim1.2{\mu}m$) oxygen inclusions played a role of forming fine acicular ferrite in the weld metal. A large amount of (Ti, Mn, Al)xOy oxygen inclusions dispersed, and oxides density was measured to be 4,600-5,300 (ea/mm2). During the welding thermal cycle, the area near a fusion line was reheated to temperature exceeding $1400^{\circ}C$. However, the nitrides and carbides were not completely dissolved near the fusion line because of rapid heating and cooling rate. Instead, they might grow during the cooling process. TiC precipitates of about 50 ~ 100nm size dispersed near the fusion line.

• Journal of the Korean Chemical Society
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• v.35 no.4
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• pp.389-396
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• 1991

The pre-concentration and determination of ultratrace arsenic in water samples was studied by the precipitate flotation technique. The arsenic in 1.0l of water sample, in which all suspended materials were filtered out, was coprecipitated together with La(OH)$_3$ precipitates at pH 8.5${\pm}$0.1. After the precipitate was made to be hydrophobic by adding mixed surfactant of 1 : 8 mole ratio of sodium oleate and sodium dodecyl sulfate, it was floated with the aid of tiny bubbles of nitrogen gas in a flotation cell. The floated precipitate was quantitatively collected on a micropore glass filter by the suction, dissolved with small volume of 1.0M sulfuric acid, and accurately diluted to 25.00ml with a de-ionized water. Total arsenic was spectrophotometrically determinated by forming silver diethyldithiocarbamate complex of arsine generated from arsenic in the concentrated solution. The calibration curve was linear up to 20ng/ml in the original solution. Analytical results showed that contents of arsenic in a campus wastewater and a river water were 8.2ng/ml and l.0ng/ml, respectively, and their recoveries were 93${\%}$ and 90${\%}$ in water samples which a given amount of arsenic was added into. From above result, it could be concluded that this method was applicable to the determination of arsenic in various kinds of water at low ng/ml levels.

• Journal of the Korean Chemical Society
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• v.35 no.4
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• pp.355-361
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• 1991

The separative preconcentration of trace mercury[Hg(II)] in a water sample was studied by a coprecipitation flotation technique. The trace Hg(II) was precipitated together with Ce(OH)$_3$ by adding 3.0 ml of 0.1M Ce$^{3+}$ solution to 1,000 ml of water sample and adjusting pH to 11.0 with 1.0M NaOH solution. The hydrophobic precipitate[Ce(OH)$_3$-Hg(OH)$_2$], which was formed by adding 2.0 ml of 0.1${\%}$ ethanolic sodium oleate solution, were floated on the surface with an aid of tiny nitrogen gas bubbles. The floated materials were quatitatively collected in a suction flask and dissolved with 5.0 ml of 2.0M HNO$_3$. The solution was marked to 25.00 ml with a deionized water. The content of Hg(II) was determined by cold vapor atomic absorption spectrophotometry. Any interferences of concomitants such as Ag$^+$, Br$^-$, I$^- $, etc. were not observed on the whole procedure. The analytical result showed that Hg(II) found in the wastewater of Seochang Campus, Korea University was 1.98 ng/ml with the relative standard deviation of 3.6${\%}$. And recoveries of Hg(II) in the wastewater into which 1.0 ng/ml and 2.0 ng/ml were added were 95${\%}$ and 91${\%}$, respectively. From such results, this procedure could be concluded to be tolerably accurate and reproducible for the determination of trace mercury in a water sample.

• Journal of the Korean Ceramic Society
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• v.50 no.6
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• pp.353-358
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• 2013

The hot corrosion behavior of plasma sprayed 4 mol% $Y_2O_3-ZrO_2$ (YSZ) thermal barrier coatings (TBCs) with volcanic ash is investigated. Volcanic ash that deposited on the TBCs in gas-turbine engines can attack the surface of TBCs itself as a form of corrosive melt. YSZ coating specimens with a thickness of 430-440 ${\mu}m$ are prepared using a plasma spray method. These specimens are subjected to hot corrosion environment at $1200^{\circ}C$ with five different duration time, from 10 mins to 100 h in the presence of corrosive melt from volcanic ash. The microstructure, composition, and phase analysis are performed using Field emission scanning electron microscopy, including Energy dispersive spectroscopy and X-ray diffraction. After the heat treatment, hematite ($Fe_2O_3-TiO_2$) and monoclinic YSZ phases are found in TBCs. Furthermore the interface area between the molten volcanic ash layers and YSZ coatings becomes porous with increases in the heat treatment time as the YSZ coatings dissolved into molten volcanic ash. The maximum thickness of this a porous reaction zone is 25 ${\mu}m$ after 100 h of heat treatment.

• Journal of the Korean Chemical Society
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• v.37 no.3
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• pp.327-333
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• 1993

A method was developed for the determination of trace elements in seawater by precipitate flotation preconcentration and subsequent flame atomic absorption detection. In order to quantitatively coprecipitate trace ions such as Cd(II), CuI(II), Fe(III), Mn(II), Pb(II) and Pd(II), 2.0 ml of 1.0M cerium(III) solution was added to 1.0l of seawater and the pH was adjusted to 9.5 with 5.0 M sodium hydroxide solution while stirring with a magnetic stirrer. The precipitate was floated with the aid of surfactant solution (1.0 ml of 0.3% sodium oleate) by bubbling nitrogen gas through a porous (No. 4) fritted glass disk. The floats was collected in a small Erlenmeyer flask by suction. The washed precipitate was dissolved in 8.0 M nitric acid and marked with deionized water in the volumetric flask of 10.0 ml. The analyte was determined by measuring the atomic absorbances in 100-fold concentrated solution. Above all analytes in Kangnung (East Sea) and Kanghwado (West Sea) sea waters were found to be under the detection limit of this method. The recoveries of over 92% for all analytes spiked into seawater samples showed that this method was applicable to the analysis of real seawater.