• Bulletin of the Korean Chemical Society
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• v.33 no.4
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• pp.1279-1284
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• 2012

Silica supported $Cs_{2.5}H_{0.5}PMo_{12}O_{40}$ catalyst was prepared through sol-gel method with ethyl silicate-40 as silicon resource and characterized by X-ray diffraction, infrared spectroscopy, scanning electron microscopy, nitrogen adsorption-desorption and potentiometric titration methods. The $Cs_{2.5}H_{0.5}PMo_{12}O_{40}$ particles with Keggin-type structure well dispersed on the surface of silica, and the catalyst exhibited high surface area and acidity. The catalytic performance of the catalysts for benzene liquid-phase nitration was examined with 65% nitric acid as nitrating agent, and the effects of various parameters were tested, which including temperature, time and amount of catalyst, reactants ratio, especially the recycle of catalyst was emphasized. Benzene was effectively nitrated to mononitro-benzene with high conversion (95%) in optimized conditions. Most importantly, the supported catalyst was proved has excellent stability in the nitration progress, and there were no any other organic solvent and sulfuric acid were used in the reaction system, so the liquid-phase nitration of benzene that we developed was an eco-friendly and attractive alternative for the commercial technology.

• Journal of the Korean Chemical Society
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• v.39 no.4
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• pp.281-287
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• 1995

Copper(Ⅱ) complexes with N,N'-oxalylbis(salicylaldehydehydrazone), N,N'-malonylbis(salicylaldehydehydrazone) and N,N'-succinylbis(salicylaldehydehydrazone) have been prepared in 95% DMF. Their protonation and stability constants were investigated by potentiometric titration. We observed that MBSH ligand showed the largest protonation constant. The values of the protonation constants among three different ligands were increased as following order SBSH < OBSH < MBSH. However, the increasing order of stability constants was somewhat different such as Cu(Ⅱ)-SBSH < Cu(Ⅱ)-MBSH < Cu(Ⅱ)-OBSH. In addition, thermodynamic parameters, ΔH and ΔS of Cu(Ⅱ) complexes have been studied. As a result, we found the SBSH ligand produced the best stable copper (Ⅱ) complex.

• Journal of the Korea Institute of Building Construction
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• v.21 no.3
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• pp.189-194
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• 2021

LIBS has been attracting attention as an analytical method capable of real-time measurement without sample preparation. In this study, a Lab. scale LIBS device was fabricated to examine the applicability and reproducibility of LIBS in the analysis of chloride contents in mortar. The existing analysis method and LIBS analysis were performed simultaneously on the mortar test specimen with the chloride content adjusted. Compared to the chloride content condition of the mortar, the XRF and Potentiometric Titration results also showed a similar trend. As a result of LIBS analysis, chlorine ions were detected at a wavelength of 837.59 nm according to the chloride content condition. In order to improve the precision in various concentration ranges, the LIBS signal amplification of about 50 times through the electric field enhancement was implemented. Through the verification of the aqueous solution-based reproducibility, a high correlation between the LIBS signal strength and the Cl concentration was confirmed, and the possibility of applying LIBS to the durability diagnosis of concrete damage by chloride was confirmed.

• Journal of the Korea institute for structural maintenance and inspection
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• v.27 no.5
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• pp.16-22
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• 2023

In this study, a salt water immersion test was performed on concrete specimens simulating the concrete mix design of the nuclear power plant, and the correlation between the amount of chloride and the XRF component according to the depth of the concrete was analyzed. The amount of chloride on the surface of the nuclear power plant concrete increased slightly with increasing immersion time in salt water, but the amount of chloride in the depth of 5.5 mm or more showed a clear tendency to increase with increasing immersion time in salt water. As a result of analyzing the correlation between the amount of chloride in concrete and the XRF component, the concrete with 20% FA substitution compared with the OPC concrete showed a very high correlation between the composition ratio of Cl ions and the evaluation result of salt damage resistance by XRF component analysis. Accordingly, it was confirmed that chlorine ion analysis and salt damage resistance performance evaluation by XRF component analysis were possible through repeated data accumulation in the nuclear power plant concrete mix with 20% fly ash replacement.

• Journal of the Mineralogical Society of Korea
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• v.25 no.4
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• pp.197-210
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• 2012

Hematite has been known to be the most stable form of various iron (oxyhydr)oxides in the surface environments. In this study, its properties as an adsorbent were examined and also adsorption of arsenic onto hematite was characterized as well. The specific surface area of hematite synthesized in our laboratory appeared to be $31.8g\;m^2/g$ and its point of zero salt effect, (PZSE) determined by potentiometric titration was observed 8.5. These features of hematite may contribute to high capacity of arsenic adsorption. From several adsorption experiments undertaken at the identical solution concentrations over pH 2~12, the adsorption of As(III) (arsenite) was greater than that of As(V) (arsenate). As of pH-dependent adsorption patterns, in addition, arsenite adsorption gradually increased until pH 9.2 and then sharply decreased with pH, whereas adsorption of arsenate was greatest at pH 2.0 and steadily decreased with the increasing pH from 2 to 12. The characteristics of these pH-dependent adsorption patterns might be caused by combined effects of the variation in the chemical speciation of arsenic and the surface charge of hematite. The experimental results on adsorption kinetics show that adsorption of both arsenic species onto hematite approached equilibrium within 20 h. Additionally, the pseudo-second-order model was evaluated to be the best fit for the adsorption kinetics of arsenic onto hematite, regardless of arsenic species, and the rate constant of As(V) adsorption was investigated to be larger than that of As(III).

• Economic and Environmental Geology
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• v.46 no.6
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• pp.521-533
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• 2013

This study was initiated to evaluate the applicability of Si slag as an adsorbent via investigation of the main properties of Si slag as an adsorbent aw well as characterization of adsorption features between aqueous arsenic and Si slag. The specific surface area of Si slag was measured to be 6.71 $m^2/g$ which seems to be slightly higher than those of other slags, but relatively lower than those of iron (oxyhydr)oxides extensively used for arsenic controlling processes. The point of zero salt effect (PZSE) of Si slag determined by potentiometric titration appeared to be comparatively high (7.3), indicating the Si slag may be favorably used for adsorption of arsenic which predominantly exists as an oxy-anions. The results of adsorption isotherm indicate that regardless of arsenic species, Langmuir-type isotherm is the most suitable to simulate the adsorption of arsenic onto Si slag. With regard to pH-dependence of arsenic adsorption, the adsorption maxima of arsenite was centered at pH 7, and the adsorption was remarkably decreased in the other pH conditions. In the case of arsenate, on the other hand, the adsorption was highest at the lowest pH (4.0) and then gradually decreased with the increase of pH. Based on the results of kinetic experiments, it is likely that the adsorption of arsenite approached equilibrium within 2 hr, but it took about 8 hr for arsenate adsorption to be equilibrated. In addition, the Pseudo second order was evaluated to be most consistent with the empirical data of arsenic adsorption onto Si slag in this study. Under identical conditions, the affinity of arsenate onto Si slag was estimated to be nearly 6 times higher than that of arsenite.

• Journal of the Korea Concrete Institute
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• v.26 no.1
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• pp.71-78
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• 2014

The long term integrity of concrete cask is very important for spent nuclear fuel dry storage system. However, there are serious concerns about early deterioration of concrete cask from creaking and corrosion of reinforcing steel by chloride ion because the cask is usually located in seaside, expecially by combined deterioration such as chloride ion and heat, carbonation. This study is to investigate the relation between temperature and chloride ion diffusion of concrete. Immersion tests using 3.5% NaCl solution that were controlled in four level of temperature, i.e. 20, 40, 65, and $90^{\circ}C$, were conducted for four months. The chloride ion diffusion coefficient of concrete was predicted based on the results of profiles of Cl- ion concentration with the depth direction of concrete specimens using the method of potentiometric titration by $AgNO_3$. Test results indicate that the diffusion coefficient of chloride ion increases remarkably with increasing temperature, and there was a linear relation between the natural logarithm values of the diffusion coefficients and the reciprocal of the temperature from the Arrhenius plots. Activation energy of concrete in this study was about 46.6 (W/C = 40%), 41.7 (W/C = 50%), 30.7 (W/C = 60%) kJ/mol under a temperature of up to $90^{\circ}C$, and concrete with lower water-cement ratio has a tendency towards having higher temperature dependency.

• Journal of the Korean Society for Marine Environment & Energy
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• v.14 no.3
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• pp.205-211
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• 2011

On board comparison of pH and total alkalinity measurement in seawater was carried out during the JES expedition on R/V Roger Revelle in the East Sea using 550 real seawater samples from the surface to the bottom. Spectrophotometry and potentiometry without liquid junction were compared for pH measurement. The pH values of two methods are generally in a good agreement. Spectrophotometry with a pipette provides higher value compare with the potentiometry in the deep layer, where pH values are lower. However, spectrophotometry without a pipette shows same values with potentiometry within their precision range. The pipetting procedure may remove of $CO_2$ in the sample, which causes increase of pH. Potentiometric titration methods using a closed-cell and an open-cell were compared for the total alkalinity measurement. Values from open cell method are smaller by about 5~10 ${\mu}mol\;kg^{-1}$ than those from closed cell method. This may be caused by the bubble formed in the closed cell during the experiment. Although any analytical method compared in this study for the pH or TA measurement can be applied, special attentions should be paid for satisfactory results.

• Korean Journal of Soil Science and Fertilizer
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• v.16 no.4
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• pp.318-324
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• 1983

Electrochemical properties of Georgia kaolinite in aqueous suspension were studied by ion adsorption, potentiometric titration, and electrophoretic mobility measurements. Kaolinite in 0.001 M and 0.1 M NaCl solution showed qualitatively both pH independent and pH depender negative and positive charges through pH range 2.5-11.0 when dissolved aluminum ions from kaolinite were considered as well as $Na^+$ and $Cl^-$ as index ions. Electrophoretic mobilities (EM) of 0.02 wt. % kaolinite suspension in distilled water and 0.001 M NaCl solution were approximately constant against mobility measuring time consumed in the electrophoresis cell at different pH values, and isoelectric points(IEP) were around pH 4.7. EM values in 0.1 M NaCl solution were positive and constant against mobility measuring time below pH 4; but above pH 4, EM values were negative for the first 10 seconds followed by positive values which became approximately constant through stepped changes after 10 minutes. Hydrated cations may bind to the six- member oxygen ring sites having multiple partial negative charges on the exterior tetrahedral layer surface by both electrostatic and hydrogen bonding force while hydrated anions bind to the partially positively charged hydrogen atoms on the exterior octahedral layer surface. Parts of the aluminol groups on the exterior octahedral layer surface as well as edge faces may be involved in complex reactions and have both anion and cation exchange capacities in the electrolyte solution above pH 4.

• Analytical Science and Technology
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• v.16 no.6
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• pp.450-457
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• 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 ($^{234}U$, $^{235}U$, $^{236}U$ 및 $^{238}U$) 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.