• Title/Summary/Keyword: Liquid phase reaction

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Development of Ternary Inorganic Binder System for Manufacturing High-Functional Ceramic Molds and Core (고기능성 세라믹 주형 및 중자 제작을 위한 3원계 무기 바인더 시스템 개발)

  • Hye-Yeong Park;Geun-Ho Cho;Hyun-Hee Choi;Bong Gu Kim;Eun-Hee Kim;SeungCheol Yang;Yeon-Gil Jung
    • Korean Journal of Materials Research
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    • v.32 no.12
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    • pp.538-544
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    • 2022
  • In existing ceramic mold manufacturing processes, inorganic binder systems (Si-Na, two-component system) are applied to ensure the effective firing strength of the ceramic mold and core. These inorganic binder systems makes it possible to manufacture a ceramic mold and core with high dimensional stability and effective strength. However, as in general sand casting processes, when molten metal is injected at room temperature, there is a limit to the production of thin or complex castings due to reduced fluidity caused by the rapid cooling of the molten metal. In addition, because sodium silicate generated through the vitrification reaction of the inorganic binder is converted into a liquid phase at a temperature of 1,000 ℃. or higher, it is somewhat difficult to manufacture parts through high-temperature casting. Therefore, in this study, a high-strength ceramic mold and core test piece with effective strength at high temperature was produced by applying a Si-Na-Ti three-component inorganic binder. The starting particles were coated with binary and ternary inorganic binders and mixed with an organic binder to prepare a molded body, and then heat-treated at 1,000/1,350/1,500 ℃ to prepare a fired body. In the sample where the two-component inorganic binder was applied, the glass was liquefied at a temperature of 1,000 ℃ or higher, and the strength decreased. However, the firing strength of the ceramic mold sample containing the three-component inorganic binder was improved, and it was confirmed that it was possible to manufacture a ceramic mold and core via high temperature casting.

Fabrication and Evaluation of a Total Organic Carbon Analyzer Using Photocatalysis

  • Do Yeon Lee;Jeong Hee Shin;Jong-Hoo Paik
    • Journal of Sensor Science and Technology
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    • v.32 no.3
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    • pp.140-146
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    • 2023
  • Water quality is crucial for human health and the environment. Accurate measurement of the quantity of organic carbon in water is essential for water quality evaluation, identification of water pollution sources, and appropriate implementation of water treatment measures. Total organic carbon (TOC) analysis is an important tool for this purpose. Although other methods, such as chemical oxygen demand (COD) and biochemical oxygen demand (BOD) are also used to measure organic carbon in water, they have limitations that make TOC analysis a more favorable option in certain situations. For example, COD requires the use of toxic chemicals, and BOD is time-consuming and can produce inconsistent and unreliable results. In contrast, TOC analysis is rapid and reliable, providing accurate measurements of organic carbon content in water. However, common methods for TOC analysis can be complex and energy-intensive because of the use of high-temperature heaters for liquid-to-gas phase transitions and the use of acid, which present safety risks. This study focuses on a TOC analysis method using TiO2 photocatalysis, which has several advantages over conventional TOC analysis methods, including its low cost and easy maintenance. For TiO2, rutile and anatase powders are mixed with an inorganic binder and spray-coated onto a glass fiber substrate. The TiO2 powder and inorganic binder solutions are adjusted to optimize the photocatalytic reaction performance. The TiO2 photocatalysis method is a simple and low-power approach to TOC analysis, making it a promising alternative to commonly used TOC analysis methods. This study aims to contribute to the development of more efficient and cost-effective approaches for water quality analysis and management by exploring the effectiveness and reliability of the developed equipment.

Structural determination of triterpenic acids in Prunellae Spica by fast atom bombardment tandem mass spectrometry (하고초의 생리활성 성분 Triterpenic Acids의 FAB-MS를 이용한 구조 규명)

  • Ahn, Young Min;Lee, Kang Ro;Hong, Jongki
    • Analytical Science and Technology
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    • v.21 no.4
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    • pp.245-258
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    • 2008
  • Five triterpenic acids as marker compounds were extracted and isolated from Prunellae Spica by column chromatography and reversed-phase high-performance liquid chromatography (HPLC), and their purity was determinated by HPLC (purity ${\geq}90%$). Molecular weight and elemental compositions of the five marker compounds were determined by fast atom bombardment high-resolution mass spectrometry (FAB-HRMS). The structural determination of the five marker compounds was carried out fast atom bombardment collision-induced dissociation tandem mass spectrometry (FAB-CID-MS/MS). The collision-induced dissociation (CID) of protonated molecules $[M+H]^+$ and deprotonated molecules $[M-H]^-$ produced diverse product ions due mainly to retro Diels-Alder reaction (RDA), dehydration and decarboxylation. Moreover, the CID-MS/MS spectra of the $[M-H]^-$ ions were observed charge-remote fragmentation (CRF) patterns. On the basis of interpretation of CID-MS/MS spectra, structural elucidation of triterpenic acids isolated from Prunellae Spica was clearly performed.

Simultaneous determination of preservatives in sausages using liquid chromatography with electrospray ionization tandem mass spectrometry (LC-MS/MS를 이용한 소시지 중 보존료 동시분석)

  • Koh, Ba-Ra-Da;Kim, Ji-Yeon;Jang, Mi-Sun;Seo, Doo-Ri;Jung, Bo-Ram;Shin, Ji-Hyun;Lim, Jin-Taek;Kim, Yong-Hwan;Kim, Eun-Sun
    • Korean Journal of Veterinary Service
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    • v.38 no.2
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    • pp.127-136
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    • 2015
  • A simultaneous determination method was developed for nine preservatives (benzoic acid, sorbic acid, dehydroacetic acid, methyl-, ethyl-, isopropyl-, propyl-, isobutyl- and butyl-parabens) in sausage by liquid chromatography with electrospray ionization tandem mass spectrometry (LC/ESI-MS/MS). Each parameter was established by multiple reaction monitoring in negative mode. Separation was achieved on a phenyl-hexyl ($2.5{\mu}m$, $2.1{\times}150mm$, Waters) with A-20 mM ammonium acetate containing 0.1% acetic acid in water, B-Acetonitrile as mobile phase with gradient mode at a flow rate of 0.3 mL/min. The developed method was validated for specificity, linearity, accuracy and precision in sausages samples. Linearity was over 0.998 with calibration curve of the mixed standards. The mean recoveries from sausages fortified at the level of 2.0~10.0 mg/L were in range of 98.60~109.16% with RSDs lower than 8.93%. The limits of detection (LOD) and the limits of quantification (LOQ) were in the range between 0.0003~0.085 mg/L and 0.01~0.257 mg/L, respectively. Intra-day precision and inter-day precision were 0.45~6.16% and 2.81~13.33%, respectively. Using presently developed determination method, 33 field sausage samples from Gwangju city in Korea were screened over nine preservatives. As a result, no preservatives were detected in all samples.

Development of Analytical Method for Colistin in Fish and Shrimp using Liquid Chromatography Mass Spectrometry (LC-MS/MS를 이용한 수산물 중 콜리스틴 분석법 개발)

  • Shin, Dasom;Kang, Hui-Seung;Lee, Soo-Bin;Cho, Yoon-Jae;Cheon, So-Young;Jeong, Jiyoon;Rhee, Gyu-Seek
    • Journal of Food Hygiene and Safety
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    • v.31 no.5
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    • pp.319-326
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    • 2016
  • Colistin is a last resort antimicrobial agent against multi-drug resistant Gram-negative bacteria. This study was conducted to develop an analytical method to determine colistin in fish and shrimp. The analytes were confirmed and quantified via liquid chromatography-tandem mass spectrometry (LC-MS/MS) in the positive ion mode using multiple reaction monitoring (MRM). The sample was extracted with acidified 5% methanol (containing 0.5% formic acid). Then, solid phase extraction (SPE) was used for cleanup. Matrix-matched calibration curves were linear over the calibration ranges (0.05-1.2 mg/kg) for all the analytes into blank sample with $r^2$ > 0.99. All the values fulfilled the criteria requested by the Codex guidelines. Average recoveries ranged from 85.9% to 107.9%. The repeatability of measurements, expressed as the coefficient of variation (CV, %), was less than 15%. The limit of detection (LOD) was 0.02 mg/kg, and the limit of quantitation (LOQ) was 0.05 mg/kg. This improved method showed higher accuracy and acceptable sensitivity to meet the CAC guideline requirements and is applicable for the analysis of residual colistin (A+B) in fish and shrimp.

Validation of an LC/MS/MS Method for the Pharmacokinetic Study of Lercanidipine (염산레르카니디핀 체내동태 연구를 위한 혈청 중 레르카니디핀의 LC/MS/MS 정량법 검증)

  • Kim, Se-Mi;Kim, Hwan-Ho;Shin, Sae-Byeok;Kang, Hyun-Ah;Yoon, Hwa;Cho, Hea-Young;Kim, Yoon-Gyoon;Yang, Chan-Woo;Yong, Chul-Soon;Lee, Yong-Bok
    • Journal of Pharmaceutical Investigation
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    • v.37 no.4
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    • pp.223-227
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    • 2007
  • A rapid, simple and sensitive LC/MS/MS method for the determination of lercanidipine in human serum was validated and applied to the pharmacokinetic study of lercanidipine. Lercanidipine and internal standard, amlodipine, were extracted from human serum by liquid-liquid extraction with hexan-isoamyl alcohol (100: 1, v/v) and analyzed on a $Symmetry^{(R)}$ MS $C_{18}$ column with the mobile phase of acetonitrile-0.2% aqueous formic acid (70: 30, v/v). Using MS/MS with multiple reaction monitoring (MRM) mode, lercanidipine and amlodipine were detected without severe interferences from human serum matrix. Lercanidipine produced a protonated precursor ion ($[M+H]^+$) at m/z 612.3 and a corresponding product ion at m/z 280.0. Internal standard produced a protonated precursor ion ($[M+H]^+$]) at m/z 409.0 and a corresponding product ion at m/z 238.0. The ruggedness of this method was investigated using quality control (QC) samples. This method showed linear response over the concentration range of 0.05-20 ng/mL with correlation coefficient greater than 0.999. The lower limit of quantitation using 0.5 mL of serum was 0.05 ng/mL, which was sensitive enough for pharmacokinetic studies. The overall accuracy of the developed method ranged from 85.51 to 112.2% for lercanidipine with overall precision (% C.V.) being 3.56-13.1%. This method showed good ruggedness (within 15% C.V.) and was successfully applied for the analysis of lercanidipine in human serum samples for the pharmacokinetic studies, demonstrating the suitability of the method.

The development and validation of a novel liquid chromatography tandem mass spectrometry (LC-MS/MS) procedure for the determination of fluoroquinolones residues in chicken muscle using modified QuEChERS (quick, easy, cheap, effective, rugged and safe) method

  • Park, Sunjin;Kim, Hyobi;Choi, Byungkook;Hong, Chung-Oui;Lee, Seon-Young;Jeon, Inhae;Lee, Su-Young;Kwak, Pilhee;Park, Sung-Won;Kim, Yong-Sang;Lee, Kwang-jick
    • Korean Journal of Veterinary Service
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    • v.42 no.4
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    • pp.289-296
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    • 2019
  • A novel rapid procedure with liquid chromatography tandem mass spectrometry (LC-MS/MS) detection has been developed by changing various conditions including sample preparation such as QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) methodology. This work has been involved the optimization and validation of detection method for fluoroquinolones which are widespread used in livestock especially in the chicken. Five grams of homogenized chicken muscle were extracted with QuEChERS EN and acetonitrile containing 5% formic acid and cleaned with anhydrous magnesium sulfate and C18 sorbent. The separation was performed on Acquity UPLC HSS T3 (2.1 mm×100 mm, 1.8 ㎛) column. The mobile phase A and B were composed of water containing 0.1% formic acid and acetonitrile containing 0.1% formic acid, respectively. Flow rate was 0.25 mL/min and column temperate was 40℃. LC-MS/MS with multiple reaction monitoring has been optimized for ten fluoroquinolones (ciprofloxacin, danofloxacin, difloxacin, enrofloxacin, marbofloxacin, norfloxacin, ofloxacin, orbifloxacin, pefloxacin and sarafloxacin). The method developed in this study has been presented good linearity with correlation coefficient (R2) of 0.9971~0.9998. LOD and LOQ values ranged from 0.09 to 0.76 ppb and from 0.26 to 2.29 ppb, respectively. The average recoveries were from 77.46 to 111.83% at spiked levels of 10.0 and 20.0 ㎍/kg. Relative standard deviation (%) ranged 1.28~11.90% on intra-day and 3.10~8.38 % on inter-day, respectively. This analysis method was applicable to the livestock residue laboratories and was expected to be satisfactory for the residue surveillance system.

Particle Behavior of Silver Nanoparticles Synthesized by Electrical Resistance Analysis (전기저항 분석을 통한 은나노 입자 합성 시의 입자거동 연구)

  • Yoon, Young Woo;Ryu, Si Hong;Yang, Sung Joo;Lee, Seong Eui
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.28 no.8
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    • pp.531-538
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    • 2015
  • This study examined the size and shape of the nano-silver particle through the analysis of electrical resistance when synthesizing nano-sized silver by using the chemical liquid reduction. Changes in particle behaviors formed according to the changes in electronic characteristics by electric resistance in each time period in the beginning of reduction reaction in a course of synthesizing the nano-silver particle formation were studied. In addition, analysis was conducted on particle behaviors according to the changes in concentration of $AgNO_3$ and in temperature at the time of reduction and nucleation and growth course when synthesizing the particles based on the particle behaviors were also examined. As the concentration of $AgNO_3$ increased, the same amount of resistance of approximately $5{\Omega}$ was increased in terms of initial electronic resistance. Furthermore, according to the result of formation of nuclear growth graph and estimation of slope based on estimated resistance, slops of $6.25{\times}10^{-3}$, $2.89{\times}10^{-3}$, and $1.85{\times}10^{-3}$ were derived from the concentrations of 0.01 M, 0.05 M, and 0.1 M, respectively. As the concentration of $AgNO_3$ increased, the more it was dominantly influenced by the nuclear growth areas in the initial phase of reduction leading to increase the size and cohesion of particles. At the time of reduction of nano-silver particle, the increases of initial resistance were $4{\Omega}$, $4.2{\Omega}$, $5{\Omega}$, and $5.3{\Omega}$, respectively as the temperature increased. As the temperature was increased into $23^{\circ}C$, $40^{\circ}C$, $60^{\circ}C$, and $80^{\circ}C$, slopes were formed as $4.54{\times}10^{-3}$, $4.65{\times}10^{-3}$, $5.13{\times}10^{-3}$, and $5.42{\times}10^{-3}$ respectively. As the temperature increased, the particles became minute due to the increase of nuclear growth area in the particle in initial period of reduction.

Determination of Nitrovin in Fishery Products by Liquid Chromatography-tandem Mass Spectrometry (LC-MS/MS를 이용한 수산물 중 니트로빈의 정량분석법 개발 및 검증)

  • Kim, Joohye;Shin, Dasom;Kang, Hui-Seung;Jeong, Jiyoon;Rhee, Gyu-Seek
    • Journal of Food Hygiene and Safety
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    • v.33 no.2
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    • pp.118-123
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    • 2018
  • The objective of this study was to develop a sensitive method for the identification and determination of nitrovin in fishery products by using a solid-phase extraction (SPE), as performed with a liquid chromatography-tandem mass spectrometry (LC-MS/MS). The samples were extracted with a mixture of acetonitrile and water, and were then defatted with acetonitrile saturated hexane, after which further clean-up was accomplished with SPE on the hydrophilic-lipophilic balance (HLB) cartridges. The analytes were subsequently ionized in the positive mode of an electrospray ionization (ESI), and where thereby detected in a process of multiple reaction monitoring (MRM). The linearity (expressed as correlation coefficients) of the matrix calibration curves was > 0.985. The limit of the quantification for the nitrovin was measured at 0.001 mg/kg. The accuracy (expressed as average recovery) was noted between 72.1 and 122%. The precision (expressed as coefficient variation) was noted from 2.9 to 16.9%. According to the CODEX CAC/GL-71 guideline accuracy, precision, linearity, and limit of detection were determined in three matrices (which were flatfish, eel and shrimp). The proposed method was suitable for analyzing the associated nitrovin residues. This application and result can also be a factor to contribute to the non-detection drugs management in fishery products.

Synthesis and Selective Gas Permeability of Liquid Crystalline Poly(allyl sulfone) Networks (액정폴리알릴술폰의 합성 및 기체 선택투과 특성)

  • Jo, Byung-Wook;Choi, Jae-Kon;Kim, Joon-Seop;Choi, Soo-Kyung
    • Elastomers and Composites
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    • v.40 no.2
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    • pp.136-142
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    • 2005
  • Liquid crystalline poly(allylsulfone) networks having $SO_2$ in a main chain and mesogens in a side chain were synthesized and their gas permeability and permselectivity were determined. The monomer II having two allyl groups on the each end group was able to form polymer networks by polymerization reaction, while the monomer I having only one allyl group was not. Molecular motion of the poly(allylsulfone) networks were retarded with increasing the cross-linking density, and the segmental motion of networks was developed enough to show isotropic phase transition. Gas permeabilities of poly(II-5 $01/I-OCH_3$ 99) were 2.58 baller for $O_2$ and 18.4 barrer for $H_2$. It means that hydrogen gas are 7 times more permeable than oxygen. Its permselectivities were high as 23.9 for ${\alpha}(H_2/N_2)$. The permselectivity was increased with increasing the cross-linking density. For example, ${\alpha}(H_2/N_2)$ was 36.8 in poly(II-5 $10/I-OCH_3$ 90), which was shown to be the highest value among these poly(allylsulfone) networks.