• Title/Summary/Keyword: Temperature separation

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Development of Isotope Dilution-Liquid Chromatography/Tandem Mass Spectrometry as a Candidate Reference Method for the Determination of Acrylamide in Potato Chips

  • Park, Sun-Young;Kim, Byung-Joo;So, Hun-Young;Kim, Yeong-Joon;Kim, Jeong-Kwon
    • Bulletin of the Korean Chemical Society
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    • v.28 no.5
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    • pp.737-744
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    • 2007
  • An isotope dilution-liquid chromatography/tandem mass spectrometric method was developed as a candidate reference method for the accurate determination of acrylamide in potato chips, starch-rich foodstuff cooked at high temperature. Sample was spiked with 13C3-acrylamide and then extracted with water. The extract was further cleaned up with an Oasis HLB solid-phase extraction (SPE) cartridge and an Oasis mixed-phase cation exchange (MCX) SPE cartridge. The extract was analyzed by using LC/ESI/Tandem MS in positive ion mode. LC with a medium reversed-phase (C4) column was optimized to obtain adequate chromatographic retention and separation of acrylamide. MS was operated to selectively monitor [M+H]+ ions of the analyte and its isotope analogue at m/z 72 and m/z 75, respectively. Sample was also analyzed by the LC/MS with selectively monitoring the collisionally induced dissociation channels of m/z 72 → m/z 55 and m/z 75 → 58. Compared to the LC/MS chromatograms, the LC/MS/MS chromatograms showed substantially reduced background chemical noises coming from solvent clusters formed during ESI spray processes and interferences from sample matrix. Repeatability and reproducibility studies showed that the LC/MS/MS method is a reliable and reproducible method which can provide a typical method precision of 1.0% while the LC/MS results are influenced by chemical interferences.

Reuse of Hydrogen Sulfide by Ferric Chelate Reaction of Food Waste Anaerobic Digestion Gas, Sulfur Recovery and its Economic Evaluation (킬레이트 착화학반응에 의한 음식물폐기물 혐기소화가스 중 황화수소의 제거와 황회수 및 경제성평가)

  • Park, Young G.;Yang, Youngsun
    • Clean Technology
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    • v.20 no.4
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    • pp.367-374
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    • 2014
  • Several experiments have been done to investigate the removal of hydrogen sulfide ($H_2S$) synthetic gas from biogas streams by means of chemical absorption and chemical reaction with 0.1-1 M Fe/EDTA solution. The roles of Fe/EDTA were studied to enhance the removal efficiency of hydrogen sulfide because of oxidizing by chelate. The motivation of this investigation is first to explore the feasibility of enhancing the toxic gas treatment in the biogas facility. The biogas purification strategy affords many advantages. For instance, the process can be performed under mild environmental conditions and at low temperature, and it removes hydrogen sulfide selectively. The end product of separation is elemental sulfur, which is a stable material that can be easily disposed with minor potential for further pollution. As the Fe-EDTA concentration increased, the conversion rate of hydrogen sulfide increased because of the high stability of Fe-EDTA complex. pH as an important environmental factor was 9.0 for the stability of chemical complex in the oxidation of hydrogen sulfide.

Imporoved Method for the Preparation of Silk Fibroin Hyoysates

  • Shukhrat Madyarov;Lee, kawng-Gill;Yeo, Joo-Hong;Jin Nam;Lee, Yong-Woo
    • Journal of Sericultural and Entomological Science
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    • v.41 no.2
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    • pp.108-115
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    • 1999
  • An improvement of methods in fibroin hydrolysates preparat significantly enlarges their applications to practical use. Acidic hydrolysis by hydrohloric acid is one of the methods for silk fibroin depolymeriza6tion. A low yield of final product and long time of the process are the demerits of this method. Possibility of preparation of water-soluble silk hydrolysates with more yield and less expenses is investigated in this study. Such possibility is occurred with the increasing tratment temperature and simultaneously decreasing treatment time, concentration of hydrochoric acid respectively, the concentration of sodium hydroxide used for neutraliza6tion of hydolysates after hydrolysis. Colour is decreased in this case and a small amount of activated, too. Protection of hydrolysates against precipitation after neutraliza6tion, and separation and during concentrating process is the other merit of this method. Creamy-coloured insoluble silk powder is the remainder of hydrolyzed fibroin. This is the only the immobiliza6tion of enzymes and other physiological active substances. Fine particles of this powder can be used as additives for artificial diets and cultural media, as well as raw materials for polymer membranes, etc.

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Base-Catalyzed Rearrangement of Some 1,3-Oxathiolane Sulfoxides: Mechanistic Viewpoint of the Sigmatropic and Elimination Reactions

  • Hahn, Hoh-Gyu;Nam, Kee-Dal;Cheon, Seung-Hoon
    • Bulletin of the Korean Chemical Society
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    • v.25 no.9
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    • pp.1379-1384
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    • 2004
  • Rearrangements of 1,3-oxathiolane sulfoxides 8 and 9 in the presence of base are described from a mechanistic viewpoint of sigmatropic and elimination reactions. In the presence of triethylamine the (Z)-sulfoxide 8 gave the corresponding thiolsulfinate 10 by way of dimerization of the sulfenic acid intermediate 2 at room temperature while the (E)-sulfoxide 9 was recovered even after refluxing in ethyl acetate by the reversal of the [2,3]-sigmatropic rearrangement of the sulfenic acid 4. Triethylamine promoted the developing charge separation in the transition state of the sigmatropic rearrangement of the (Z)-sulfoxide 8 to facilitate the ring opening to the sulfenic acid 2. The reason for more facile ring opening of the (Z)-sulfoxide 8 in comparison with the corresponding (E)-sulfoxide 9 is attributable to the differences in the reactivity of the hydrogen adjacent to the carbonyl group. Triethylamine was not strong base to deprotonate the carbonyl-activated methylene hydrogen of the (E)-sulfoxide 9 but enough to catalyze the sigmatropic process of the sulfoxides. The sulfenic acid 2 dimerized to the thiolsulfinate 10 while the sulfenic acid 4 proceeded the sigmatropic ring closure. In the presence of strong base such as potassium hydroxide, the elimination reaction was predominant over the sigmatropic rearrangement. In this reaction condition, both sulfoxides 8a and 9a gave a mixture of the disulfide 12, the isomeric disulfide 14, and the sulfinic acid 13. Under the strong alkaline condition an elimination of activated hydrogen from the carbon adjacent to the carbonyl group to furnish the sulfenic acid 2a and the isomeric sulfenic acid 18. The formation of the transient intermediate in the reaction was proven by isolation of the isomeric disulfide 14. The reactive entity was regarded as the sulfenic acid rather than sulfenate anion under these reaction conditions.

Synthesis of Silica/Alumina Composite Membrane Using Sol-Gel and CVD Method for Hydrogen Purification at High Temperature (Sol-gel 및 CVD법을 이용한 고온 수소 분리용 silica/alumina 복합막의 합성)

  • 서봉국;이동욱;이규호
    • Membrane Journal
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    • v.11 no.3
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    • pp.124-132
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    • 2001
  • Silica membranes were prepared on a porous ${\alpha}$-alumina tube with pore size of 150nm by sol-gel and chemical vapor deposition(CVD) method for hydrogen separation at high temperatures. Silica and ${\gamma}$-lumina membranes formed by the sol-gel method possessed a large amount of mesopores of a Knudsen diffusion regime. In order to improve the $H_2$ selectivity, silica was deposited in the sol-gel derived silica/${\gamma}$-alumina layer by thermal decomposition of tetraethyl orthosilicate(TEOS) at $600^{\circ}C$. The CVD with forced cross flow through the porous wall of the support was very effective in plugging mesopores that were left unplugged in the membranes. The CVD modified silica/alumina composite membrane completely rejected nitrogen permeation and thus showed a high $H_2$ selectivity by molecular sieve effect. the permeation of hydrogen was explained by activated diffusion and the activation energy was 9.52kJ/mol.

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The Community Structure of Phytoplankton in Winter and Summer Around Wangdol-cho (동해 왕돌초 주변 해역의 동계와 하계 식물플랑크톤 군집 분포)

  • Shim, Jeong-Min;Jin, Hyun-Gook;Sung, Ki-Tack;Hwang, Jae-Dong;Yun, Suk-Hyun;Lee, Yong-Hwa;Kim, Young-Suk;Kwon, Ki-Young
    • Journal of Environmental Science International
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    • v.17 no.12
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    • pp.1403-1411
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    • 2008
  • Wangdol-cho, located 23 km offshore of Hupo in southwest of East Sea, is underwater rock floor, called to Wangdol-Am or Wangdol-Jam and has three tops as Mat-Jam, Middle-Jam and Set-Jam. The composition, abundance, diversity and community structure were investigated in winter and summer in 2002 around Wangdol-cho. The temperature around the Northwest and Southeast part of Wangdol-cho was influenced by the North Korea Cold Current (NKCC) and East Korea Warm Current (EKWC), respectively. Nutrient and chlorophyll-a concentration were higher at the top of Wangdol-cho than other area. A total of 41 genera and 78 species of phytoplankton were identified. The average cell abundance of phytoplankton in winter and summer were $286{\times}10^3\;cells/m^3,\;432{\times}10^3\;cells/m^3$ respectively. The largest community was Bacillariophyta containing 52 taxa. The dominant species were Lauderia anulata and Coscinodiscus spp. which preferred cold water in winter. In contrast, warm water species such as Rhizosolenia stolterfothii and Ceratium spp. were dominant in summer. The average species diversity index of phytoplankton in winter was higher than that in summer. According to dominant species and standing crops, phytoplankton community resulted in a clear separation. One group was western area, which showed low density, and the other was eastern area, which showed the higher density. The abundance and species composition of phytoplankton. were affected by topological characteristics around Wangdol-cho.

Isothermal Vapor-Liquid Equilibria at 333.15K and Thermodynamic Excess Properties for the Binary System of Methanol+Dimethyl Carbonate (Methanol+Dimethyl Carbonate 혼합계의 333.15 K 등온 기-액 평형과 열역학 과잉 물성)

  • Han, Kyu-Jin;Park, So-Jin
    • Korean Chemical Engineering Research
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    • v.43 no.3
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    • pp.387-392
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    • 2005
  • Recently, dimethyl carbonate (DMC) is considered as an alternative of MTBE (methyl tert-butyl ether), additive for non-leaded gasoline with their fast biodegradation rate and low toxicity. DMC is usually synthesized so far by oxidative carbonylation of methanol, and recently developed synthetic process is also started with methanol. Since the phase equilibria of the system, consisted of DMC and methanol or other reaction products on different temperature and pressure is necessary for the optimum separation process design and operation. However the reported phase equilibria and physical properties for DMC mixtures in the Dortmund Data Bank (DDB; thermodynamic property data bank) are quite rare. Besides, infinitely dilute properties are not found. In this work, isothermal vapor-liquid equilibria at 333.15 K for methanol+DMC binary system and mixing properties, excess molar volume and viscosity deviation at 298.15 K are directly measured and correlated. Additionally, infinitely dilute activity coefficient of methanol in the DMC solvent at three different temperatures are measured and compared with predicted values using modified UNIFAC (Dortmund).

Equilibrium, Kinetic and Thermodynamic Parameter Studies on Adsorption of Acid Yellow 14 Using Activated Carbon (활성탄을 이용한 Acid Yellow 14 흡착에 대한 평형, 동역학 및 열역학 파라미터의 연구)

  • Lee, Jong Jib
    • Korean Chemical Engineering Research
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    • v.54 no.2
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    • pp.255-261
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    • 2016
  • Adsorption experiments of Acid Yellow 14 dye using activated carbon were carried out as function of adsorbent dose, pH, initial concentration, contact time and temperature. The equilibrium adsorption data were analyzed by Langmuir, Freundlich and Temkin isotherm model. The experimental data were best represented by Freundlich isotherm model. Base on the estimated Freundlich constant (1/n=0.129~0.212) and Langmuir separation factor ($R_L=0.202{\sim}0.243$), this process could be employed as effective treatment method. The heat of adsorption of Temkin isotherm model was 5.101~9.164 J/mol indicated that the adsorption process followed a physical adsorption. Adsorption kinetics experimental data were modeled using the pseudo-first-order and pseudo-second-order kinetic equation. It was shown that pseudo-second-order kinetic equation could best describe the adsorption kinetics. Base on the negative Gibbs free energy (-4.81~-10.33 kJ/mol) and positive enthalpy (+78.59 kJ/mol) indicate that the adsorption is spontaneous and endothermic process.

Comparative studies for the performance of a natural gas steam reforming in a membrane reactor (분리막 반응기를 이용한 천연가스 개질반응의 성능에 관한 비교 분석)

  • Lee, Boreum;Lim, Hankwon
    • Journal of the Korean Institute of Gas
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    • v.20 no.6
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    • pp.95-101
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    • 2016
  • For a natural gas steam reforming, comparative studies of the performance in a conventional packed-bed reactor and a membrane reactor, a new conceptual reactor consisting of a reactor with series of hydrogen separation membranes, have been performed. Based on experimental kinetics reported by Xu and Froment, a process simulation model was developed with Aspen $HYSYS^{(R)}$, a commercial process simulator, and effects of various operating conditions like temperature, $H_2$ permeance, and Ar sweep gas flow rate on the performance in a membrane reactor were investigated in terms of reactant conversion and $H_2$ yield enhancement showing improved $H_2$ yield and methane conversion in a membrane reactor. In addition, a preliminary cost estimation focusing on natural gas consumption to supply heat required for the system was carried out and feasibility of possible cost savings in a membrane reactor was assessed with a cost saving of 10.94% in a membrane reactor.

Degradation of Organic Component in MSW by Super-heated Steam (과열(過熱) 증기(蒸氣)를 이용한 국내 폐기물(廢棄物) 유기성(有機性) 성분의 분해(分解) 특성 연구)

  • Kim, Woo-Hyun;Roh, Seon-Ah;Min, Tai-Jin;Sung, Hyun-Je;Park, Seong-Bum;Jang, Ha-Na
    • Resources Recycling
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    • v.18 no.6
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    • pp.10-17
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    • 2009
  • Degradation of the organic component in the waste were carried out by superheated steam in a pressurized vessel. The effects of waste characteristics, reaction temperature and residence time on the degradation rate have been determined. The biodegradable organic components such as food and paper waste have been degraded, and plastics, wood and metal were remained without degradation. The degradation efficiency is decided by the desizing rate of the waste, and the waste mixture with 23% biodegradable organic component shows higher desizing rate than that of the 43% of the biodegradable organic component in a short residence time and the desizing rate is found to be 90% in the maximum condition.