• Title/Summary/Keyword: system separation method

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Development of HPLC Determination Method for Trace Levels of 1-, 2-Nitropyrenes and 2-Nitrofluoranthene in Airborne Particulates and Its Application to Samples Collected at Noto Peninsula

  • Hayakawa, Kazuichi;Tang, Ning;Sato, Kosuke;Izaki, Akihiko;Tatematsu, Michiya;Hama, Hirotaka;Li, Ying;Kameda, Takayuki;Toriba, Akira
    • Asian Journal of Atmospheric Environment
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    • v.5 no.3
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    • pp.146-151
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    • 2011
  • 1-Nitropyrene (1-NP), 2-NP and 2-nitrofluoranthene (2-NFR) are useful markers for studying the atmospheric behaviors of polycyclic aromatic hydrocarbons (PAHs) and nitropolycyclic aromatic hydrocarbons (NPAHs). However, present methods for measuring trace levels of these compounds are lesssensitive and laborious. Here we describe several improvements to a previously reported high-performance liquid chromatography-chemiluminescence detection system that allows it to determine trace levels of 1-, 2-NPs and 2-NFR. The proposed system was equipped with a reducer column packed with Pt/Rh instead of zinc whose life-time was limited. The combination of Cosmosil MS-II (monomeric ODS) and AR-II (polymeric ODS) columns was used instead of polymeric ODS columns as the separator column to improve the separation. An ethanol mixture with acetate buffer (pH 5.5) was used in place of an acetonitrile mixture with the same buffer to activate the reducer column. The same ethanol mixture was used as the mobile phase for the clean-up column. The switching time of the column switching valve was optimized to concentrate the amino-derivatives of above NPAHs quantitatively on the concentrator column. The concentrations of bis(2,4,6-trichlorophenly) oxalate and hydrogen peroxide in the chemiluminescence reagent solution were optimized to 0.4 mM and 30 mM, respectively, to increase the sensitivity. Under the above conditions, the detection limits (S/N=3) of 1-, 2-NPs and 2-NFR were 1 fmol (0.25 pg), 10 fmol (2.5 pg) and 4 fmol (1 pg), respectively. The proposed system was effectively used to determine trace levels of 1-, 2-NPs and 2-NFR in airborne particulates collected at Noto Peninsula. The atmospheric concentrations of 1-, 2-NPs and 2-NFR were not more than sub pg $m^{-3}$ levels. They were higher in winter (January) than in summer (July). In both seasons, the concentrations were in decreasing order, [2-NFR]>[1-NP]>[2-NP].

Effects of Oxalic and L-ascorbic acids on Iron Removal form Iron-bearing Illite (일라이트 분체 내에 함유된 산화철 제거에 옥살산과 L-아스코르브산이 미치는 영향)

  • Lee, Won-Pyo;Kang, Il-Mo;Moon, Hi-Soo
    • Economic and Environmental Geology
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    • v.40 no.2 s.183
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    • pp.141-151
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    • 2007
  • This study was focused on iron removal from illite by L-ascorbic and oxalic acids. Iron has been shown as a secondary mineral such as iron oxides and hydroxides in illite ores. It is also known as a primary agent to degrade brightness index of the ores. Methods such as physical separation and chemical leaching with strong inorganic acids have been widely used to remove the iron from the ores. However, these methods are expensive and give rise to environmental problems. In this study, we examined an alternative method using solutions with different set of combination of sulfuric, hydrochloric, L-ascorbic, and oxalic acids. Compared to chemical treatments with only inorganic acids, our results demonstrate that an addition of L-ascorbic acid in inorganic acids results in decreasing both total concentrations of the inorganic acids and time for the treatments. The treatment with 0.15 M L-ascorbic acid and 0.25 M sulfuric acid in solution for 60 min significantly improved the brightness index from 42.4% to 74.4%. This improvement is similar to that of treatment with only 2.5 M sulfuric acid alone for 150 min. Mineralogical and chemical analyses were performed to compare the effect of acid leaching on illite powders. No obvious differences are observed in the mineralogical characteristics and particle size distributions of the samples. These results suggest that the treatment with the addition of L-ascorbic acid in sulfuric acid could effectively remove iron without modifying the physicochemical properties of illite under conditions used in this study.

A Study on the New Development for Determination of Dead Time in GC-OTC/FID (GC-OTC/FID에서 Dead Time 결정을 위한 새로운 방법 개발에 대한 연구)

  • Oh, Doe Seok;Kim, Sung Wha;Ko, Eun Ah;Jeon, Hyung Woo
    • Journal of the Korean Chemical Society
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    • v.63 no.4
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    • pp.246-252
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    • 2019
  • In the system of GC-OTC/FID (Gas chromatography-Open Tubular Column/Flame Ionization Detector), DMSO (Dimethyl sulfide) solvent was used to separate the polar solvents (Alcohols). In this system DMSO was eluted later than the separated polar solvents. At this system to calculate chromatographic factors [adjusted retention time ($t_R^{\prime}=t_R-t_O$), capacity factor{$k^{\prime}=(t_R-t_O)/t_O$} and separation factor {${\alpha}=(t_{R2}-t_O)/(t_{R1}-t_O)$}], dead time($t_O$) is necessary, but the method to calculate it has not been reported yet. Therefore, we have tried to develop $t_O$. To calculate $t_O$, we conversed DMSO retention time (DMSO $t_R$) to logarithm ($f(x)={\log}\;t_{R(DMSO)}{\rightarrow}t_O$, $t_O={\log}$ 9.551=0.980). To confirm the optimization of the developed method, we compared with $CH_4\;t_R$ and ${\ln}\;t_{R(DMSO)}$. Both of the values calculated by $CH_4\;t_R$ and ${\ln}\;t_{R(DMSO)}$ were not suitable in the calculation k' and ${\alpha}$. The developed method in this study{${\log}\;t_{R(DMSO)}$} has satisfied both of the values k' criteria (1${\alpha}(1<{\alpha}<2)$. The developed calculation method in this study was easy and convenient, therefore it can be expected to be applied to these similar systems.

Study of Polysulfone Membrane for Membrane-covered Oxygen Probe System (산소 전극 시스템에 사용되는 polysulfone막에 대한 연구)

  • Hong, Suk In;Kim, Hyun Joon;Park, Hee Young;Kim, Tae Jin;Jeong, Yong Seob
    • Applied Chemistry for Engineering
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    • v.7 no.5
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    • pp.877-887
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    • 1996
  • The ideal membranes for membrane-covered oxygen probes system should be selectively permeable for oxygen and chemically inert, and have good mechanical strength. Polysulfone(PSf) was selected to develop the membrane for membrane-covered oxygen electrodes system. PSf membranes have properties such as good reproducibility, good mechanical strength, chemical inertness, and high heat resistance. PSf membranes were cast from polymer solution on the glass plate at constant temperature, and casting solvents used were tetrahydrofuran(THF), methylene chloride, and N-methyl-2-pyrrolidone(NMP). Tricresyl phosphate(TCP) as plasicizer was added to PSf to increase the softness of membrane. The permeation characteristics were observed for pure oxygen and nitrogen through pure PSf membranes by variable volume method and membrane-covered electrode system. The permeability coefficients of oxygen and nitrogen measured by variable volume method were slightly decreased with increasing of upstream pressure. The permeation properties of PSf membrane using methylene choride as casting solvent were not affected by the PSf amount of polymer solution. The permeability coefficients of oxygen and nitrogen for PSf membrane containing TCP were very slightly lower than those for pure PSf membrane, but ideal separation factors were slightly higher. The flexibility of PSf membrane containing 2wt% TCP was better than that of pure PSf membrane. It was expected that this increase in flexibility would solve the difficulty of fixing the membrane to the cathode. The membrane-covered oxygen probes system was composed of anode, cathode and electrolyte. The type of the anode was Ag/AgCl half-cell, that of cathode was Ag, and the electrolyte was 4N KCl solution. The result of sampled current voltametry for PSf membrane showed the plateu region at -0.3V~-1.0V. The correlation coefficient of oxygen partial pressure versus current for PSf membrane was relatively high, 0.99949. It was concluded that PSf membrane was the good candidate for the membrane-covered oxygen probes system.

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Determination of Four Macrolide Antibiotics Residues in Chicken Muscle Using High-Performance Liquid Chromatography (액체크로마토그래피를 이용한 닭고기 시료에서의 마크로라이드계 동시분석법 개발)

  • Lee, Sang-Hee;Yoo, Miyoung;Shin, Dong-Bin
    • Journal of Food Hygiene and Safety
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    • v.28 no.1
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    • pp.19-23
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    • 2013
  • A simple and rapid method has been developed and validated for simultaneous determination of each macrolides residues (spiramycin, josamycin, tilmicosin, tylosin) in chicken muscle by high-performance liquid chromatography- photo diode array (HPLC-PDA). Chicken muscle sample have been extracted with liquid-liquid extraction process; analytes was extracted by acetonitrile, and then defatted with hexane saturated by acetonitrile. The HPLC separation was performed on a Unison UK-$C_{18}$ ($150mm{\times}3.0mm$, $3{\mu}m$) with a gradient system of 0.1% trifloroacetic acid (TFA) and 0.1% trifloroacetic acid (TFA) in acetonitrile as the mobile phase. The drugs were detected at 232 nm for spiramycin and josamycin, and 287 nm for tilmicosin and tylosin. The limits of quantification (LOQs) were between 27 and $59{\mu}g/kg$; and the intra- and inter-day precision (relative standard deviation; RSD) was between 0.9-13.2 and 2.4-13.1%, respectively in chicken muscle sample. The method may has been successfully applied for multiresidue determination of four macrolides below the maximum residue limits (MRLs) established by the European Union (EU).

Effects of In Vitro Maturation, In Vitro Fertilization and In Vitro Culture Conditions on Bovine Embryo Production (체외성숙, 수정 및 배양에 있어서 각기 다른 배양조건들이 소 체외수정란의 생산에 미치는 효과)

  • 조성근;송상현;공일근;이효종;최상용;박충생
    • Journal of Embryo Transfer
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    • v.15 no.1
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    • pp.67-75
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    • 2000
  • This study was conducted to establish the optimal conditions for in vitro embryo production using oocytes derived from follicles of slaughter-house ovaries. The ovaries of Hanwoo were obtained from a local slaughter-house. The oocytes were aspirated from visible follicles of 2~7mm in diameter. The recovered oocytes which were completely surrounded by at least 2 layers of cumulus cells and a homogeneous cytoplasmic pigmentation were used. The selected oocytes were washed 3 or 4 times with D-PBS containing 10% bovine calf serum (BCS) and matured in vitor (IVM) in Ham's F-10 supplemented with 10% BCS or 0.01 $\mu\textrm{g}$/ml epidermal growth factor(EGF) at 39$^{\circ}C$ under 5% CO2 in air for 24 hours. They were fertilizqed in vitro (IVF) with fresh sperm separated by Percoll density gradient or swim-up in TALP media. The zygotes were cultrued with or without bovine oviductal epitherial cells(BOEC) in media(HECM-6 supplemented with 11 amino acid and / or TCM-199 supplemented with 10% BCS) for 7 to 10 days. The results obtained were as follow: The cleavage rate and developmental rate to blastocyst after maturation and IVF were not significantly different between Ham's F-10 with EGF(76.0% vs. 44.0%) and BCS(75.9% vs. 43.6%)(P<0.05). The cleavage rate and development rate to blastocyst after fertilizing by swim-up or Percoll method were not signifciantly(P<0.05) different between swim-up (80.2% vs. 29.2%) and Percoll(81.9% vs. 26.5%) (P<0.05). The cleavage rate in TCM 199(80.5) was signficiantly higher than that in HECM-6 (72.0%) (P<0.05). However, developmental rate to blastocyst using TCM 199 following HECM-6 for 3 or 4 days (42.2%) was significantly higher than that in TCM-199 alone(26.7%)(P<0.05). The cleavage rate and development rate of embryos produced in vitro by exchange timing for HECM-6 media were not significantly different between in day 3(78.6% vs. 45.5%) and day 4(75.0% vs. 43.2%)(P<0.05). The cleavage rate and developmental rate to blastocysts according to co-culture system were not significantly different between with (74.2% vs. 41.4%) and without BOEC(73.95 vs. 43.5%) (P<0.05). The number of blastomere in blastocyst stage after co-culture with or without BOEC was not significantly different (106.7$\pm$5.1 and 96.6$\pm$4.0). In conclusion, the most transferable IVP embryos could be produced from Ham's F-10 medium for IVM, Percoll density gradient method for IVF sperm separation and in vitro culture in HECM-6 until day 3 or day 4, and then transferred into TCM-199 until day 9 within adequate embryo density in culture droplets after insemination.

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Isolation of Ginsenoside${-Rh}_1$ and ${-Rh}_2$ by High Performance Liquid Chromatography (고속액체(高速液體) 크로마토그래피에 의(依)한 Ginsenoside ${-Rh}_1$${-Rh}_2$ 의 분리(分離))

  • Choi, Jin-Ho;Kim, Woo-Jung;Hong, Soon-Keun;Oh, Sung-Ki;Oura, Hikokichi
    • Korean Journal of Food Science and Technology
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    • v.13 no.1
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    • pp.57-66
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    • 1981
  • An effective method for isolation of the major components of ginseng saponin such as $ginsenoside-Rb_{1},\;-Rb_2,$ -Rc, -Rd, -Re and $-Rg_1$, and the minor components such as ginsenoside-Rf, $-Rg_2,\;and-Rh_1$, was developed and reported in previous papers (J. Korean Agr. Chem. Soc., 23(4), 199 and 206(1980) The conditions and procedures used for isolation and identification for ginsenosides described in the previous papers were not sufficient enough for clean separation of minor components, $ginsenoside-Rh_1,\;and-Rh_2$. In this work, modifications in extraction method and in mobile phase for HPLC were attempted. It was found that application of ethyl acetate extraction at $60^{\circ}C$ for 3 hr on crude saponin resulted in a removal of diol group saponin from crude saponin which made it possible for using higher portion of acetonitrile in mobile phase. The mixed solvents of acetonitrile : water (92 : 8 and 94 : 6) gave excellent resolution of $ginsenoside-Rh_1\;and\;-Rh_2$.

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Study of Spin Jig Development for Cleaning of the PCB component (PCB기판 세척용 스핀 지그개발에 관한 연구)

  • Lee, Seung-Chul;Park, Suk-Chul
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.15 no.8
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    • pp.4736-4741
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    • 2014
  • This study examined PCB component cleaning on a PCB component surface, which has defects of precipitation type washing (existing rinse method), sealant and foreign material formed in the adhesive process that could not be removed easily. The spin jig was developed for PCB component cleaning, in which the PCB component settled down, to solve the conventional problem of the removal of foreign material with the centrifugal force by high speed rotation. The results are as follows. With decreasing fraction defect in PCB component washing, the development and substrate damage decreased by more than 80% according to the abstergent in the rotary type using the centrifugal force in the existing precipitation type. When the base plate showed a large difference with the time to include the process after washing the design using the existing method, easy attachment and separation of the PCB component could be possible. The washing time was enhanced 90% compared to the existing time. The reliability of the security and washing collaboration of the design and stability of the cleaning process could be secured so that there was no phenomenon of secession, the PCB component fixed for a cleansing rotation jig could maintain a fixed force by the centrifugal force. The stability and reliability of the washing process and the defective rate could be improved to less than 1%.

A study on the lip shape recognition algorithm using 3-D Model (3차원 모델을 이용한 입모양 인식 알고리즘에 관한 연구)

  • 배철수
    • Journal of the Korea Institute of Information and Communication Engineering
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    • v.3 no.1
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    • pp.59-68
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    • 1999
  • Recently, research and developmental direction of communication system is concurrent adopting voice data and face image in speaking to provide more higher recognition rate then in the case of only voice data. Therefore, we present a method of lipreading in speech image sequence by using the 3-D facial shape model. The method use a feature information of the face image such as the opening-level of lip, the movement of jaw, and the projection height of lip. At first, we adjust the 3-D face model to speeching face image sequence. Then, to get a feature information we compute variance quantity from adjusted 3-D shape model of image sequence and use the variance quality of the adjusted 3-D model as recognition parameters. We use the intensity inclination values which obtaining from the variance in 3-D feature points as the separation of recognition units from the sequential image. After then, we use discrete HMM algorithm at recognition process, depending on multiple observation sequence which considers the variance of 3-D feature point fully. As a result of recognition experiment with the 8 Korean vowels and 2 Korean consonants, we have about 80% of recognition rate for the plosives and vowels. We propose that usability with visual distinguishing factor that using feature vector because as a result of recognition experiment for recognition parameter with the 10 korean vowels, obtaining high recognition rate.

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The Design and Implementation of Ontology for Simulation based Architecture Framework (ONT-AF) in Military Domain (SBA AF의 구축을 지원하는 온톨로지의 설계 및 구현(ONT-SAF))

  • Kwon, Youngmin;Sohn, Mye;Lee, Wookey
    • Journal of Information Technology and Architecture
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    • v.9 no.3
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    • pp.233-241
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    • 2012
  • Architecture framework (AF) is a guideline to define components needed to develop and operate enterprise architecture (EA), and to define relationships among the components. There are many architecture frameworks to operate EA of governments and businesses such as Zachman framework, DoDAF, TOGAF, FEAF, and TEAF. DoDAF is the most representative AF to support the development of the EA in the military domain. DoDAF is composed of eight viewpoints and 40 views that are affiliated with the viewpoints. To develop an AF for a specific goal, system architects decide a set of views. Furthermore, they determine data that are needed for a view modeling. However, views and data in DoDAF are structurally inter-related explicitly and/or implicitly. So, developing an AF for a specific goal is going to be a project to be carried out over a long haul. To reduce the burden of its development, in this paper, we develop ONT-SAF (Ontology for DoDAF) that can infer inter-relationships like referential and transitive relationships and the sequences among the views. Furthermore, to promote reusability and consistency of the views and the data within an AF, we adopt the view-data separation strategy. ONT-DAT contains classes like 'viewpoint', 'view', 'data', 'expression method', and 'reference model', and 11 properties including 'hasView.' To prove the effectiveness of ONT-SAF, we perform a case study.