• Journal of Soil and Groundwater Environment
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• v.14 no.3
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• pp.1-13
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• 2009

Alkalinity and total carbon contents were measured by acid neutralizing titration (ANT), back titration (BT), gravitational weighing (GW), non-dispersive infrared-total carbon (NDIR-TC) methods for assessing precision and accuracy of alkalinity and total carbon concentration in $CO_2$-rich water. Artificial $CO_2$-rich water(ACW: pH 6.3, alkalinity 68.8 meq/L, $HCO_3^-$ 2,235 mg/L) was used for comparing the measurements. When alkalinity measured in 0 hr, percent errors of all measurement were 0~12% and coefficient of variation were less than 4%. As the result of post-hoc analysis after repeated measure analysis of variance (RM-AMOVA), the differences between the pair of methods were not significant (within confidence level of 95%), which indicates that the alkalinity measured by any method could be accurate and precise when it measured just in time of sampling. In addition, alkalinity measured by ANT and NDIR-TC were not change after 24 and 48 hours open to atmosphere, which can be explained by conservative nature of alkalinity although $CO_2$ degas from ACW. On the other hand, alkalinity measured by BT and GW increased after 24 and 48 hours open to atmosphere, which was caused by relatively high concentration of measured total carbon and increasing pH. The comparison between geochemical modeling of $CO_2$ degassing and observed data showed that pH of observed ACW was higher than calculated pH. This can be happen when degassed $CO_2$ does not come out from the solution and/or exist in solution as $CO_{2(g)}$ bubble. In that case, $CO_{2(g)}$ bubble doesn't affect the pH and alkalinity. Thus alkalinity measured by ANT and NDIR-TC could not detect the $CO_2$ bubble although measured alkalinity was similar to the calculated alkalinity. Moreover, total carbon measured by ANT and NDIR-TC could be underestimated. Consequently, it is necessary to compare the alkalinity and total carbon data from various kind of methods and interpret very carefully. This study provide technical information of measurement of dissolve $CO_2$ from $CO_2$-rich water which could be natural analogue of geologic sequestration of $CO_2$.

• Clean Technology
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• v.25 no.1
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• pp.81-90
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• 2019

A dielectric barrier discharge (DBD) plasma reactor packed with $Ni-CeO_2/{\gamma}-Al_2O_3$ catalyst was used for the dry ($CO_2$) reforming of propane (DRP) to improve the production of syngas (a mixture of $H_2$ and CO) and the catalyst stability. The plasma-catalytic DRP was carried out with either thermally or plasma-reduced $Ni-CeO_2/{\gamma}-Al_2O_3$ catalyst at a $C_3H_8/CO_2$ ratio of 1/3 and a total feed gas flow rate of $300mL\;min^{-1}$. The catalytic activities associated with the DRP were evaluated in the range of $500{\sim}600^{\circ}C$. Following the calcination in ambient air, the ${\gamma}-Al_2O_3$ impregnated with the precursor solution ($Ni(NO_3)_2$ and $Ce(NO_3)_2$) was subjected to reduction in an $H_2/Ar$ atmosphere to prepare $Ni-CeO_2/{\gamma}-Al_2O_3$ catalyst. The characteristics of the catalysts were examined using X-ray diffraction (XRD), transmission electron microscopy (TEM), field emission scanning electron microscopy (FE-SEM), energy dispersive X-ray spectrometry (EDS), temperature programmed reduction ($H_2-TPR$), temperature programmed desorption ($H_2-TPD$, $CO_2-TPD$), temperature programmed oxidation (TPO), and Raman spectroscopy. The investigation revealed that the plasma-reduced $Ni-CeO_2/{\gamma}-Al_2O_3$ catalyst exhibited superior catalytic activity for the production of syngas, compared to the thermally reduced catalyst. Besides, the plasma-reduced $Ni-CeO_2/{\gamma}-Al_2O_3$ catalyst was found to show long-term catalytic stability with respect to coke resistance that is main concern regarding the DRP process.

• Korean Journal of Heritage: History & Science
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• v.47 no.4
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• pp.224-243
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• 2014

This study examined the materials and casting technology(cast, alloy, etc.) used in the manufacturing of bronze artifacts based on old literature such as Yongjae Chonghwa, Cheongong Geamul, and The Korea Review. In the casting experiment for restoration of Sangpyong Tongbo, a bronze and brass mother coin mold was made using the sand mold casting method described in The Korea Review. The cast was comprised of the original mold plate frame, wooden frame, and molding sand. Depending on the material of the outer frame, which contains the molding sand, the original mold plate frame can be either a wooden frame or steel frame. For the molding sand, light yellow-colored sand of the Jeonbuk Iri region was used. Next, the composition of the mother alloy used in the restoration of Sangpyong Tongbo was studied. In consideration of the evaporation of tin and lead during actual restoration, the composition of Cu 60%, Zn 30%, and Pb 10% for brass as stated in The Korea Review was modified to Cu 60%, Zn 35%, and Pb 15%. For bronze, based on the composition of Cu 80%, Sn 6%, and Pb 14% used for Haedong Tongbo, the composition was set as Cu 80%, Sn 11%, and Pb 19%. The mother coin mold was restored by first creating a wooden father coin, making a cast from the wooden frame and basic steel frame, alloying, casting, and making a mother coin. Component analysis was conducted on the mother alloy of the restored Sangpyong Tongbo, and its primary and secondary casts. The bronze mother alloy saw a 5% increase in copper and 4% reduction in lead. The brass parent alloy had a 5% increase in copper, but a 4% and 12% decrease in lead and tin respectively. Analysis of the primary and secondary mother coin molds using an energy dispersive spectrometer showed that the bronze mother coin mold had a reduced amount of lead, while the brass mother coin mold had less tin. This can be explained by the evaporation of lead and tin in the melting of the primary mother coin mold. In addition, the ${\alpha}$-phase and lead particles were found in the mother alloy of bronze and brass, as well as the microstructure of the primary and secondary coin molds. Impurities such as Al and Si were observed only in the brass mother coin mold.

• Journal of Food Hygiene and Safety
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• v.34 no.2
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• pp.140-147
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• 2019

An analytical method was developed for the determination of quinoxyfen in agricultural products using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method by liquid chromatography-tandem mass spectrometry (LC-MS/MS). The samples were extracted with 1% acetic acid in acetonitrile and water was removed by liquid-liquid partitioning with $MgSO_4$ (anhydrous magnesium sulfate) and sodium acetate. Dispersive solid-phase extraction (d-SPE) cleanup was carried out using $MgSO_4$, PSA (primary secondary amine), $C_{18}$ (octadecyl) and GCB (graphitized carbon black). The analytes were quantified and confirmed by using LC-MS/MS in positive mode with MRM (multiple reaction monitoring). The matrix-matched calibration curves were constructed using six levels ($0.001-0.25{\mu}g/mL$) and the coefficient of determination ($R^2$) was above 0.99. Recovery results at three concentrations (LOQ, 10 LOQ, and 50 LOQ, n=5) were in the range of 73.5-86.7% with RSDs (relative standard deviations) of less than 8.9%. For inter-laboratory validation, the average recovery was 77.2-95.4% and the CV (coefficient of variation) was below 14.5%. All results were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and Food Safety Evaluation Department guidelines (2016). The proposed analytical method was accurate, effective and sensitive for quinoxyfen determination in agricultural commodities. This study could be useful for the safe management of quinoxyfen residues in agricultural products.

• Journal of Food Hygiene and Safety
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• v.34 no.2
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• pp.115-123
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• 2019

An analytical method was developed for the determination of fenpropimorph, a morpholine fungicide, in hulled rice, potato, soybean, mandarin and green pepper using QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) sample preparation and LC-MS/MS (liquid chromatography-tandem mass spectrometry). The QuEChERS extraction was performed with acetonitrile followed by addition of anhydrous magnesium sulfate and sodium chloride. After centrifugation, d-SPE (dispersive solid phase extraction) cleanup was conducted using anhydrous magnesium sulfate, primary secondary amine sorbents and graphitized carbon black. The matrix-matched calibration curves were constructed using seven concentration levels, from 0.0025 to 0.25 mg/kg, and their correlation coefficient ($R^2$) of five agricultural products were higher than 0.9899. The limits of detection (LOD) and quantification (LOQ) were 0.001 and 0.0025 mg/kg, respectively, and the limits of quantification for the analytical method were 0.01 mg/kg. Average recoveries spiked at three levels (LOQ, $LOQ{\times}10$, $LOQ{\times}50$, n=5) and were in the range of 90.9~110.5% with associated relative standard deviation values less than 5.7%. As a result of the inter-laboratory validation, the average recoveries between the two laboratories were 88.6~101.4% and the coefficient of variation was also below 15%. All optimized results were satisfied the criteria ranges requested in the Codex guidelines and Food Safety Evaluation Department guidelines. This study could serve as a reference for safety management relative to fenpropimorph residues in imported and domestic agricultural products.

• Journal of the Korean Electrochemical Society
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• v.24 no.4
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• pp.120-132
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• 2021

Although the development of high-Nickel is being actively carried out to solve the capacity limitation and the high price of raw cobalt due to the limitation of high voltage use of the existing LiCoO₂, the deterioration of the battery characteristics due to the decrease in structural stability and increase of the Ni content. It is an important cause of delaying commercialization. Therefore, in order to increase the high stability of the Ni-rich ternary cathod material LiNi_0.6Co_0.2Mn_0.2O₂, precursor Ni_0.6Co_0.2Mn_0.2-x(OH)₂/xTiO₂ was prepared using a nanosized TiO₂ suspension type source for uniform Ti substitution in the precursor. It was mixed with Li₂CO₃, and after heating, the cathode active material LiNi_0.6Co_0.2Mn_0.2-xTi_xO₂ was synthesized, and the physical properties according to the Ti content were compared. Through FE-SEM and EDS mapping analysis, it was confirmed that a positive electrode active material having a uniform particle size was prepared through Ti-substituted spherical precursor and Particle Size Analyzer and internal density and strength were increased, XRD structure analysis and ICP-MS quantitative analysis confirmed that the capacity was effectively maintained even when the Ti-substituted positive electrode active material was manufactured and charging and discharging were continued at high temperature and high voltage.

• Korean Journal of Environmental Agriculture
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• v.41 no.2
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• pp.82-94
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• 2022

BACKGROUND: Spiropidion and its metabolite are tetramic acid insecticide and require the establishment of an official analysis method for the safety management because they are newly registered in Korea. Therefore, this study was to determine the analysis method of residual spiropidion and its metabolite for the five representative agricultural products. METHODS AND RESULTS: Three QuEChERS methods (original, AOAC, and EN method) were applied to optimize the extraction method, and the EN method was finally selected by comparing the recovery test and matrix effect results. Various adsorbent agents were applied to establish the clean up method. As a result, the recovery of spiropidion was reduced when using the dispersive-SPE method with MgSO₄, primary secondary amine (PSA), graphitized carbon black (GCB) and octadecyl (C₁₈) in soybean. Color interference was minimized by selecting the case including GCB and C18 in addition to MgSO₄. This method was established as the final analysis method. LC-MS/MS was used for the analysis by considering the selectivity and sensitivity of the target pesticide and the analysis was performed in MRM mode. The results of the recovery test using the established analysis method and inter laboratory validation showed a valid range of 79.4-108.4%, with relative standard deviation and coefficient of variation were less than 7.2% and 14.4%, respectively. CONCLUSION(S): Spiropidion and its metabolite could be analyzed with a modified QuEChERS method, and the established method would be widely available to ensure the safety of residual insecticides in Korea.

• Korean Journal of Mineralogy and Petrology
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• v.35 no.2
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• pp.111-123
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• 2022

Carbonate green rust (CGR) and sulfate green rust (SGR) commonly occur in nature. In this study, CGR and SGR were synthesized through co-precipitation, and their formation mechanisms and physicochemical properties were investigated. X-ray diffraction (XRD) and Rietveld refinement showed both CGR and SGR with layered double hydroxide structure were successfully synthesized without any secondary phases under each synthetic condition. Refined structural parameters (unit cell) for two green rusts were a (=b) = 3.17 Å and c = 22.52 Å for CGR and a (=b) = 5.50 Å and c = 10.97 Å for SGR with the crystallite size 57.8 nm in diameter from (003) reflection and 40.1 nm from (001) reflections, respectively. Scanning electron microscopy/energy dispersive X-ray spectroscopy (SEM/EDS) results showed that both CGR and SGR had typical hexagonal plate-like crystal morphologies but their chemical composition is different in the content of C and S. In addition, Fourier transform infrared (FT-IR) spectroscopy analysis revealed that carbonate (CO₃^2-) and sulfate (SO₄^2-) molecules were occupied as interlayer anions of CGR and SGR, respectively. These SEM/EDS and FT-IR results were in good agreement with XRD results. Changes in the solution chemistry (i.e., pH, Eh and residual iron concentrations (Fe(II):Fe(III)) of the mixed solution) were observed as a function of the injection time of hydroxyl ion (OH^-) into the iron solution. Three different stages were observed in the formation of both CGR and SGR; precursor, intermediator, and green rust in the formation of both CGR and SGR. This study provides co-precipitation methods for CGR and SGR in a way of the stable synthesis. In addition, our findings for the formation mechanisms of the two green rusts and their physicochemical properties will provide crucial information with researches and industrials in utilizing green rust.

• Journal of the Korean Chemical Society
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• v.66 no.2
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• pp.78-85
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• 2022

Natural white clay was treated with 6 M of H₂SO₄ and heated at 80℃ for 6 h under mechanical stirring and the resulting acid active clay was used as an adsorbent for the removal of Cs⁺ in water. The physicochemical changes of natural white clay and acid active clay were observed by X-ray Fluorescence Spectrometry (XRF), BET Surface Area Analyser and Energy Dispersive X-line Spectrometer (EDX). While activating natural white clay with acid, the part of Al₂O₃, CaO, MgO, SO₃ and Fe₂O₃ was dissolved firstly from the crystal lattice, which bring about the increase in the specific surface area and the pore volume as well as active sites. The specific surface area and the pore volume of acid active clay were roughly twice as high compared with natural white clay. The adsorption of Cs⁺ on acid active clay was increased rapidly within 1 min and reached equilibrium at 60 min. At 25 mg L^- of Cs⁺ concentration, 96.88% of adsorption capacity was accomplished by acid active clay. The adsorption data of Cs⁺ were fitted to the adsorption isotherm and kinetic models. It was found that Langmuir isotherm was described well to the adsorption behavior of Cs⁺ on acid active clay rather than Freundlich isotherm. For adsorption Cs⁺ on acid active clay, the Langmuir isotherm coefficients, Q, was found to be 10.52 mg g^-1. In acid active clay/water system, the pseudo-second-order kinetic model was more suitable for adsorption of Cs⁺ than the pseudo-first-order kinetic model owing to the higher correlation coefficient R² and the more proximity value of the experimental value q_e,exp and the calculated value q_e,cal. The overall results of study showed that acid active clay could be used as an efficient adsorbent for the removal of Cs⁺ from water.

• Korean Journal of Heritage: History & Science
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• v.55 no.3
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• pp.120-129
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• 2022

The purpose of this study is to analyze the chemical composition of smalt pigments used in 10 large Buddhist paintings in the Joseon Dynasty using energy dispersive X-ray spectroscopy, and to clarify the material and characteristics by observing morphological characteristics using polarized light microscopy and a scanning electron microscope. Through chemical composition analysis, the smalt of all 10 large Buddhist paintings is judged to be potash glass using SiO₂ as a former and K₂O as a flux. In addition to the components related to cobalt ore used as a colorant, the paintings were found to contain high levels of As₂O₃, BaO, and PbO. The smalt particles did not have specific forms, and were blue in color, with various chromaticity. In some particles, conchoidal fracture, spherical bubbles, and impurities were observed. Through backscattered electron images, it was found that the smalt from paintings produced in the early 18th century AD had a high level of As, but the smalt from paintings produced from the mid-18th century AD onwards exhibited various contrast differences from particle to particle, and there was smalt with high levels of As, Ba, and Pb. Through the above results, the large Buddhist paintings in the Joseon Dynasty are divided into three smalt types. Type A is a type with high As₂O₃, type B is a type with high BaO, and type C is a type with high PbO. Looking at the three types of smalt pigments by the period of production, although some in-between periods were not detected, type A was confirmed to have been used from 1705 to 1808, while type B and type C were shown to have appeared in 1750 and used until 1808. This reveals that only one type of smalt was used until the early 18th century AD, and from the middle of the 18th century AD, several types of smalt were mixed and used in one large Buddhist painting. Studies such as this research are expected to provide insights into the characteristics of the smalt pigments used to produce large Buddhist paintings at the time.