• Title/Summary/Keyword: Liquid phase reaction

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Some considerations for the determination of carbonyl compounds in air: Reaction characteristics of formaldehyde with 2.4-DNPH (대기 중 카보닐 계열 성분의 분석기법의 연구: 포름알데하이드와 DNPH의 반응 특성을 중심으로)

  • Hong, Y.J.;Kim, K.H.
    • Analytical Science and Technology
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    • v.18 no.1
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    • pp.43-50
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    • 2005
  • A number of carbonyl compounds including formaldehyde and acetaldehyde are well known for their toxicity and irritancy. Hence, acquisition of both qualitative and quantitative tool for their analysis is essential to resolve issues associated with malodor or indoor pollution. Using HPLC/UV method, we examined various aspects involved in the measurements of formaldehyde in environmental samples. The results of our analysis indicated that its detection was made as low as 0.5 ppb (assuming 5 L of sample volume), while its precision was maintained near 2% in terms of relative standard error (RSE). When the stability of calibration was checked by variability of slope values obtained over long-term period (e.g., one month), its values were found to remain constantly with RSE values of 3%. It was also found that liquid-phase reaction between formaldehyde and DNPH proceed very slowly to attain equilibrium (one and half hour), while requiring adequate amount of DNPH to form their derivatives. The overall results of our study thus suggest that there are a number of factors to consider for the accurate analysis of formaldehyde in ambient air.

Determination of Formaldehyde in Cosmetics Using a Convenient DNPH Derivatization Procedure Followed by HPLC Analysis (간편한 DNPH 유도체화 HPLC 분석법을 이용한 화장품 중 포름알데하이드 분석)

  • Choi, Jongkeun
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.42 no.1
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    • pp.65-73
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    • 2016
  • Korea Food and Drug Administration (KFDA) has officially announced 2,4-dinitrophenylhydrazine (DNPH) derivatization - high performance liquid chromatography (HPLC) methods for analysis of formaldehyde. This study was conducted to develop a convenient derivatization method for cosmetics by improving complex pre-treatment procedures included in KFDA method. To simplify pre-treatment procedures of KFDA method, reaction conditions including pH, time and temperature were optimized. This pre-treatment method does not require complicate pre-treatment steps of KFDA method such as pH adjustment of test solution with acetate buffer (pH 5.0), solvent-solvent partitioning with dichloromethane and concentrating procedure with vacuum evaporator. Formaldehyde-dinitrophenylhydrazone (formaldehyde-DNP) product produced by derivatization reaction was separated and quantified with a reversed-phase HPLC, which was slightly modified with KFDA method. The linearity test showed good results with 0.9999 of correlation coefficient ($r^2$) in the range of 2 ~ 40 ppm of standard solutions. In this method, limit of detection (LOD) and limit of quantitation (LOQ) values for formaldehyde were 0.2 ppm and 0.5 ppm, respectively. In addition, recovery test demonstrated that the method was also accurate and reproducible. Therefore, the proposed method can be applicable to rapid analysis of formaldehyde in cosmetics.

Thermoelectric Efficiency Improvement in Vacuum Tubes of Decomposing Liquid Lithium-Ammonia Solutions (진공튜브 속에서 분해하는 리튬암모니아 솔루션의 열전효율 향상)

  • Lee, Jungyoon;Kim, Miae;Shim, Kyuchol;Kim, Jibeom;Jeon, Joonhyeon
    • Korean Chemical Engineering Research
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    • v.51 no.3
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    • pp.358-363
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    • 2013
  • Lithium-ammonia (Li-$NH_3$) solutions are possible to be successfully made under the vacuum condition but there still remains a problem of undergoing stable and reliable decomposition in vacuum for high-efficiency thermoelectric power generation. This paper describes a new method for improving the thermoelectric conversion efficiency of Li-$NH_3$ solutions in vacuum. The proposed method uses a 'U'-shaped Pyrex vacuum tube for the preparation and decomposition of pure fluid Li-$NH_3$ solutions. The tube is shaped so that a gas passageway ('U') connecting both legs of the 'U' helps to balance pressure inside both ends of the tube (due to $NH_3$ gasification) during decomposition on the hot side. Thermoelectric experimental results show that solution reaction in the 'U'-shaped tube proceeds more stably and efficiently than in the 'U'-shaped tube, and consequently, thermoelectric conversion efficiency is improved. It is also proved that the proposed method can provide a reversible reaction, which can rotate between synthesis and decomposition in the tube, for deriving the long-time, high-efficiency thermoelectric power.

Alternative Immunossays

  • Barnard, G.J.R.;Kim, J.B.;Collins, W.P.
    • Korean Journal of Animal Reproduction
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    • v.9 no.2
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    • pp.133-139
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    • 1985
  • An immunoassay may be defined as an analytical procedure involving the competitive reaction between a limiting concentration of specific antibody and two populations of antigen, one of which is labelled or immobillized. The advent of immunoassay has revolutionised our knowledge of reproductive physiology and the practice of veterinary and clinical medicine. Radioimmunoassay (RIA) was the first of these methods to be developed, which meausred the analyte with good sensitivity, accuracy and precision (1,2). The essential components of RIA are:-(i) a limited concentration of antibodies, (ii) a reference preparation, and (iii) an antigen labelled with a radioisotope (usually tritium or iodine-125). Most procedures invelove isolating the antibody-bound fraction and measuring the amount of labelled antigen. Good facilities are available for scintilltion counting, data reduction nd statistical analysis. RIA is undergoing refinement through:-(i) the introduction of new techniques to separate the antibody-bound and free fractions which minimize the misclassification of labelled antigen into these compartments, and the amount of non-specfic binding. (3), (ii) the development of non-extration for the measurement of haptens (4), (iii) the determination of a, pp.rent free (i.e. non-protein bound) analytes (5), and (iv) the use of monoclonal antibodies(6). In 1968, Miles and Hales introduced in important new type of immunoassay which they termed immunora-diometric assay (IRMA) based on t도 use of isotopically labelled specific antibodies(7) in a move from limited to excess reagent systems. The concept of two-site IRMAs (with a capture antibody on a solid-phase, and a second labelled antibody to a different antigenic determinant of the analyte) has enabled the development of more sensitive and less-time consuming methods for the measurement of protein hormones ovar wide concentration of analyte (8). The increasing use of isotopic methos for diverse a, pp.ications has exposed several problems. For example, the radioactive half-life and radiolysis of the labelled reagent limits assay sensitivity and imposes a time limit on the usefulness of a kit. In addition, the potential health hazards associated with the use and disposal of radioactive cmpounds and the solvents and photofluors necessary for liquid scientillation counting are incompatable with the development of extra-laboratory tests. To date, the most practical alternative labels to radioisotopes, for the measurement of analytes in a concentration > 1 ng/ml, are erythrocytes, polystyrene particiles, gold sols, dyes and enzymes or cofactors with a visual or colorimetric end-point(9). Increased sensitivity to<1 pg/ml may be obtained with fluorescent and chemiluminescent labels, or enzymes with a fluorometric, chemiluminometric or bioluminometric end-point. The sensitivity of any immunoassay or immunometric assay depends on the affinity of the antibody-antigen reaction, the specific activity of the label, the precision with which the reagents are manipulated and the nonspecific background signal (10). The sensitivity of a limited reagent system for the measurement of haptens or proteins is mainly dependent upon the affinity of the antibodies and the smalleest amount of reagent that may be manipulated. Consequently, it is difficult in practice to improve on the sensitivity obtained with iodine-125 as the label. Conversely, with excess reagent systems for the measurement of proteins it is theoretically possible to increase assay sensitivity at least 1000 fold with alternative luminescent labels. To date, a 10-fold improvement has been achieved, and attempts are being made to reduce the influence of other variables on the specific signal from the immunoreaction.

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Analysis of clenbuterol in bovine muscle and milk by LC-ESI/MS/MS (LC-ESI/MS/MS를 이용한 소고기와 우유에서의 클렌부테롤 분석)

  • Hong, Selyung;Jeong, Jiyoon;Park, Hyejin;Lee, Soonho;Lee, Jongok
    • Analytical Science and Technology
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    • v.21 no.6
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    • pp.535-542
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    • 2008
  • A liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI/MS/MS) method was developed for the determination and confirmation of clenbuterol in bovine muscle and milk. Clenbuterol and clenbuterol-D9 using as an internal standard in samples were extracted with ethyl acetate after hydrolysis and evaporated to dryness. The extracts were dissolved in 20% methanol and cleaned using HLB solid-phase extraction cartridge. The analytes were detected by LC-ESI/MS/MS on a $C_{18}$ column. Mass spectral acquisition was done in selected reaction monitoring (SRM) in positive ion mode to provide a high degree of sensitivity. Using MS/MS with SRM mode, the transitions (precursor to product) monitored were m/z 277${\rightarrow}$203 for clenbuterol, and m/z 286${\rightarrow}$204 for internal standard. The limits of quantitation (LOQ) and mean recoveries of clenbuterol in bovine muscle were $0.2{\mu}g/kg$ and 84.3~91.1%, respectively. The LOQ and mean recoveries in milk were $0.05{\mu}g/kg$ and 87.7~98.3%, respectively.

Solid state reactive sintering of cold pressed thermoelectric Mg3Sb2 (냉간 압축 성형한 Mg3Sb2 열전재료의 고상 반응 소결)

  • Kim, In-Ki;Jang, Kyung-Wook;Oh, Han-Jun
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.24 no.4
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    • pp.176-182
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    • 2014
  • We intended to prepare $Mg_3Sb_2$ compound bodies through solid state reactive sintering after cold-pressing mixtures of elementary Mg and Sb powders and investigated the crystal phases of the sintered bodies according to Mg/Sb mole ratios and reaction temperatures. The $Mg_3Sb_2$ bodies sintered at the temperatures of 773~843 K showed typical crystalline phases of $Mg_3Sb_2$ compounds, but their diffraction angles in XRD patterns were slightly different along with the vertical axis of the bodies obtained. All the bottom parts of the sintered $Mg_3Sb_2$ bodies were composed of the typical crystalline phases of $Mg_3Sb_2$ compounds and their diffraction angles were completely in accord with those of the ${\alpha}-Mg_3Sb_2$ phase, when Mg : Sb = 3.15 : 1.85 at 823 K, or when the Mg moles were greater than or equal to 3.10 at 843 K. It was considered that the slightly remaining Mg phases were formed by precipitation from ${\alpha}-Mg_3Sb_2$ phases during the solidification process of liquid phase.

The Study on the Analysis Method of Tetrodotoxin in Puffer Fish (복어 중 테트로도톡신 분석법에 관한 연구)

  • Kang, Young-Woon;Lee, Yoon-Suk;Park, Sung-Kug;Seo, Jung-Heok;Kim, Mee-Hye
    • Journal of Food Hygiene and Safety
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    • v.27 no.1
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    • pp.37-41
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    • 2012
  • The current standard for testing tetrodotoxin (TTX) in foodstuffs is the mouse bioassay (MBA) in Korea as in many other countries. However, this test suffers from potential ethical concerns over the use of live animals. In addition, the mouse bioassay does not test for a specific toxin thus a sample resulting in mouse incapacitation would need further confirmatory testing to determine the exact source toxin (e.g., TTX, STX, brevotoxin, etc.). Furthermore, though the time of death is proportional to toxicity in this assay, the dynamic range for this proportional relationship is small thus many samples must be diluted and new mice be injected to yield a result that falls within the quantitative dynamic range. Therefore, in recent years, there have been many efforts in this field to develop alternative assays. High performance liquid chromatography (HPLC) coupled with mass spectrometry (MS) has been emerged as one of the most promising options. A LC-MS-MS method involves solid-phase extraction (SPE) and followed by analysis using an electrospray in the positive ionization mode and multiple reactions monitoring (MRM). To adopt LC-MS-MS method as alternative standard for testing TTX, we performed a validation study for the quantification of TTX in puffer fish. This LC-MS-MS method showed good sensitivity as limits of detection (LOD) of $0.03{\sim}0.08{\mu}g/g$ and limits of quantification (LOQ) of $0.10{\sim}0.25{\mu}g/g$. The linearity ($r^2$) of tetrodotoxin were 0.9986~0.9997, the recovery were 80.9~103.0% and the relative standard deviations (RSD) were 4.3~13.0%. The correlation coefficient between the mouse bioassay and LC/MS/MS method was higher than 0.95.

A Review on Electrochemical Model for Predicting the Performance of Lithium Secondary Battery (리튬이차전지 성능 모사를 위한 전기화학적 모델링)

  • Yang, Seungwon;Kim, Nayeon;Kim, Eunsae;Lim, Minhong;Park, Joonam;Song, Jihun;Park, Sunho;Appiah, Williams Agyei;Ryou, Myung-Hyun;Lee, Yong Min
    • Journal of the Korean Electrochemical Society
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    • v.22 no.1
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    • pp.43-52
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    • 2019
  • As the application area of lithium secondary batteries becomes wider, performance characterization becomes difficult as well as diverse. To address this issue, battery manufacturers have to evaluate many batteries for a longer period, recruit many researchers and continuously introduce expensive equipment. Simulation techniques based on battery modeling are being introduced to solve such difficulties. Various lithium secondary battery modeling techniques have been reported so far and optimal techniques have been selected and utilized according to their purpose. In this review, the electrochemical modeling based on the Newman model is described in detail. Particularly, we will explain the physical meaning of each equation included in the model; the Butler-Volmer equation, which represents the rate of electrode reaction, the material and charge balance equations for each phase (solid and liquid), and the energy balance. Moreover, simple modeling processes and results based on COMSOL Multiphysics 5.3a will be provided and discussed.

An Estimation of Concentration of Asian Dust (PM10) Using WRF-SMOKE-CMAQ (MADRID) During Springtime in the Korean Peninsula (WRF-SMOKE-CMAQ(MADRID)을 이용한 한반도 봄철 황사(PM10)의 농도 추정)

  • Moon, Yun-Seob;Lim, Yun-Kyu;Lee, Kang-Yeol
    • Journal of the Korean earth science society
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    • v.32 no.3
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    • pp.276-293
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    • 2011
  • In this study a modeling system consisting of Weather Research and Forecasting (WRF), Sparse Matrix Operator Kernel Emissions (SMOKE), the Community Multiscale Air Quality (CMAQ) model, and the CMAQ-Model of Aerosol Dynamics, Reaction, Ionization, and Dissolution (MADRID) model has been applied to estimate enhancements of $PM_{10}$ during Asian dust events in Korea. In particular, 5 experimental formulas were applied to the WRF-SMOKE-CMAQ (MADRID) model to estimate Asian dust emissions from source locations for major Asian dust events in China and Mongolia: the US Environmental Protection Agency (EPA) model, the Goddard Global Ozone Chemistry Aerosol Radiation and Transport (GOCART) model, and the Dust Entrainment and Deposition (DEAD) model, as well as formulas by Park and In (2003), and Wang et al. (2000). According to the weather map, backward trajectory and satellite image analyses, Asian dust is generated by a strong downwind associated with the upper trough from a stagnation wave due to development of the upper jet stream, and transport of Asian dust to Korea shows up behind a surface front related to the cut-off low (known as comma type cloud) in satellite images. In the WRF-SMOKE-CMAQ modeling to estimate the PM10 concentration, Wang et al.'s experimental formula was depicted well in the temporal and spatial distribution of Asian dusts, and the GOCART model was low in mean bias errors and root mean square errors. Also, in the vertical profile analysis of Asian dusts using Wang et al's experimental formula, strong Asian dust with a concentration of more than $800\;{\mu}g/m^3$ for the period of March 31 to April 1, 2007 was transported under the boundary layer (about 1 km high), and weak Asian dust with a concentration of less than $400\;{\mu}g/m^3$ for the period of 16-17 March 2009 was transported above the boundary layer (about 1-3 km high). Furthermore, the difference between the CMAQ model and the CMAQ-MADRID model for the period of March 31 to April 1, 2007, in terms of PM10 concentration, was seen to be large in the East Asia area: the CMAQ-MADRID model showed the concentration to be about $25\;{\mu}g/m^3$ higher than the CMAQ model. In addition, the $PM_{10}$ concentration removed by the cloud liquid phase mechanism within the CMAQ-MADRID model was shown in the maximum $15\;{\mu}g/m^3$ in the Eastern Asia area.

Heterogeneous Oxidation of Liquid-phase TCE over $CoO_x/TiO_2$ Catalysts (액상 TCE 제거반응을 위한 $CoO_x/TiO_2$ 촉매)

  • Kim, Moon-Hyeon;Choo, Kwang-Ho
    • Journal of Korean Society of Environmental Engineers
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    • v.27 no.3
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    • pp.253-261
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    • 2005
  • Catalytic wet oxidation of ppm levels of trichloroethylene (TCE) in water has been conducted using $TiO_2$-supported cobalt oxides at a given temperature and weight hourly space velocity. 5% $CoO_x/TiO_2$ might be the most promising catalyst for the wet oxidation at $36^{\circ}C$ although it exhibited a transient behavior in time on-stream activity. Not only could the bare support be inactive for the wet decomposition reaction, but no TCE removal also occurred by the process of adsorption on $TiO_2$ surface. The catalytic activity was independent of all particle sizes used, thereby representing no mass transfer limitation in intraparticle diffusion. Characterization of the $CoO_x$ catalyst by acquiring XPS spectra of both fresh and used Co surfaces gave different surface spectral features of each $CoO_x$. Co $2p_{3/2}$ binding energy of Co species exposed predominantly onto the outermost surface of the fresh catalyst appeared at 781.3 eV, which is very similar to the chemical states of $CoTiO_x$ such as $Co_2TiO_4$ and $CoTiO_3$. The spent catalyst possessed a 780.3 eV main peak with a satellite structure at 795.8 eV. Based on XPS spectra of reference Co compound, the TCE-exposed Co surfaces could be assigned to be in the form of mainly $Co_3O_4$. XRD measurements indicated that the phase structure of Co species in 5% $CoO_x/TiO_2$ catalyst even before reaction is quite comparable to the diffraction lines of external $Co_3O_4$ standard. A model structure of $CoO_x$ present on titania surfaces would be $Co_3O_4$, encapsulated in thin-film $CoTiO_x$ species consisting of $Co_2TiO_4$ and $CoTiO_3$, which may be active for the decomposition of TCE in a flow of water.