• Title/Summary/Keyword: SPE1

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Optimization of solid phase extraction and simultaneous determination of trace anions in concentrated hydrofluoric acid by ion chromatography (불산 중 극미량 음이온 분석을 위한 고상 추출법 및 이온크로마토그래프를 이용한 동시분석법 확립)

  • Yoon, Suk-Hwan;Jo, Dong-ho;Kim, Hyun-Ji;Shin, Ho-Sang
    • Analytical Science and Technology
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    • v.29 no.5
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    • pp.219-224
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    • 2016
  • 불산 중 극미량 음이온의 고상추출과 이온크로마토그래프를 이용한 고감도 분석법이 개발되었다. 불산 중 불소이온이 고상에 의해 제거하였고 이어서 음이온 (F, CH3COO, Cl, Br, NO3, PO43−, SO42−)들이 이온크로마토그래프를 이용하여 연속적으로 분리하였다. 고상 추출법에 영향을 주는 각 인자들 (흡착제의 선택, 시료의 부피 및 pH, 용출 용액과 용출용액의 부피)을 결정하였으며 그 결과 흡착제로서 Oasis WAX 컬럼이 가장 우수하였고 1.0 mL의 시료부피, 용출용액으로 50 mM 초산암모늄염 5 mL가 분리능에서 가장 우수하였다. 개발한 방법에 의한 음이온 (Cl, Br, NO3, PO43−, SO42−)들의 방법검출한계는 25 % 불산용액 (w/w) 중에 0.04~0.30 µg/L의 범위를 보였고 정밀도는 20.0와 40.0 µg/L의 농도에서 5 % 이내를 보였다. 한 제조회사에 의한 25 % 불산 중 음이온의 4.2에서 47.5 µg/L의 범위로 모두 검출되었다. 이 방법은 시험절차가 간단하고, 재현성 및 감도가 좋아서 반도체회사에서 불산 중 음이온 불순물을 정도 관리하는데 매우 유용한 방법이 될 것으로 판단된다.

Three-Phase Eulerian Computational Fluid Dynamics (CFD) of Air-Water-Oil Separator with Coalescer (유적 합체기가 포함된 공기-물-기름 분리 공정에 대한 3상 Eulerian 전산유체역학)

  • Lim, Young-Il;Le, Thuy T.;Park, Chi-Kyun;Lee, Byung-Don;Kim, Byung-Gook;Lim, Dong-Ha
    • Korean Chemical Engineering Research
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    • v.55 no.2
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    • pp.201-213
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    • 2017
  • Water is removed from crude oil containing water by using oil separator. This study aims to develop a three-dimensional (3D) Eulerian computational fluid dynamics (CFD) model to predict the separation efficiency of air-water-oil separator. In the incompressible, isothermal and unsteady-state CFD model, air is defined as continuous phase, and water and oil are given as dispersed phase. The momentum equation includes the drag force, lift force and resistance force of porous media. The standard k-${\varepsilon}$ model is used for turbulence flow. The exit pressures of water and oil play an important role in determining the liquid level of the oil separator. The exit pressures were identified to be 6.3 kPa and 5.1 kPa for water and oil, respectively, to keep a liquid level of 25 cm at a normal operating condition. The time evolution of volume fractions of air, water and oil was investigated. The settling velocities of water and oil along the longitudinal separator distance were analyzed, when the oil separator reached a steady-state. The oil separation efficiency obtained from the CFD model was 99.85%, which agreed well with experimental data. The relatively simple CFD model can be used for the modification of oil separator structure and finding optimal operating conditions.

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.

Simultaneous Determination and Occurrences of Pharmaceuticals by Solid-Phase Extraction and Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS) in Environmental Aqueous Samples

  • Koo, So-Hyun;Jo, Cheon-Ho;Shin, Sun-Kyoung;Myung, Seung-Woon
    • Bulletin of the Korean Chemical Society
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    • v.31 no.5
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    • pp.1192-1198
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    • 2010
  • Pharmaceuticals and personal care products (PPCPs) are emerging contaminants in the aquatic environment. Many pharmaceuticals are not completely removed during wastewater treatment, leading to their presence in wastewater treatment effluents, rivers, lakes, and ground water. Here, we developed analytical methods for monitoring ten pharmaceuticals from surface water by LC/ESI-MS/MS. For sample clean-up and extraction, MCX (mixed cation exchange) and HLB (hydrophilic-lipophilic balance) solid-phase extraction (SPE) cartridges were used. The limits of detection (LOD) in distilled water and the blank surface water were in the range of 0.006 - 0.65 and 1.66 - 45.05 pg/mL, respectively. The limits of quantitation (LOQ) for the distilled water and the blank surface water were in the range of 0.02 - 2.17 and 5.52 - 150.15 pg/mL, respectively. The absolute recoveries for fortified water samples were between 62.1% and 125.4%. Intra-day precision and accuracy for the blank surface water were 2.9% - 24.1% (R.S.D.) and -16.3% - 16.3% (bias), respectively. In surface wastewater near rivers, chlortetracycline and acetylsalicylic acid were detected frequently in the range of 0.017 - 5.404 and 0.029 - 0.269 ng/mL, respectively. Surface water near rivers had higher levels than surface water of domestic treatment plants.

Purification and Characterization of an $\alpha$ -L-Arabinofuranosidase from Bacillus sp. DSNC 101 (Bacillus sp. DSNC 101이 생산하는 $\alpha$-L-Arabinofuranosidase의 정제 및 특성)

  • 조남철;진종언
    • The Korean Journal of Food And Nutrition
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    • v.14 no.1
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    • pp.65-68
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    • 2001
  • ${\alpha}$-L-Arabinofuranosidase was purified from the culture supernatant of Bacillus sp. DSNC 101. The enzyme had a molecular weight of 56 kDa. Optimum temperature and pH for ${\alpha}$-L-arabinofuranosidase activity were 55$^{\circ}C$ and 7.0 respectively. The Michaelis constant(Km) and maximal reaction velo-city(Vmax) for p-nitrophenyl-${\alpha}$-L-arabinofuranoside were 1.0 mM and 113.6 U/mg protein, respe-ctively. ${\alpha}$-L-Arabinofuranosidase was completely inhibited by HgCl$_2$ and CuSO$_4$. The enzyme was spe-cific for the ${\alpha}$-linked arabinoside in the furanoside configuration. The enzyme was produced during growth on agricultural residue such as rice straw, but not during growth on spelt xylan, glucose or cellobiose.

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Investigation of Domoic acid in Shellfish Collected from Korean Fish Retail Outlets

  • Choi, Kyu-Duck;Lee, Jong-Soo;Lee, Jong-Ok;Oh, Keum-Soon;Shin, Il-Shik
    • Food Science and Biotechnology
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    • v.18 no.4
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    • pp.842-848
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    • 2009
  • The purpose of this study was to determine the extent of domoic acid (DA) a potent neurotoxin, responsible for the syndrome amnesic shellfish poisoning (ASP) contamination of various species of bivalve shellfish purchased from fish market in Korea and the implications for food safety. Liquid chromatography (LC) methods were applied to quantify DA in shellfish after sample clean-up using solid-phase extraction (SPE) with strong anion exchange (SAX) cartridges. Toxin detection was achieved using photodiode array ultraviolet (LC-UV) and electrospray ionization-mass (LC-ESI-MS). DA was identified in 4 bivalve shellfishes of 872 shellfishes collected from March, 2006 to October, 2007 in Korea. DA amount of 3 surf clams (Mactra veneriformis) collected at Seoul, Daejeon, and Daegu were 4.13, 1.99, and 1.94 mg/kg, respectively. DA amount of 1 pink butterfly shell (Peronidia venulosa) collected at Seoul was 3.02 mg DA/kg. The amounts of DA that were present in 4 bivalve shellfishes were within EU guideline limits for sale of shellfish (20 mg DA/kg).

Determination of Acaricides in Honey by Solid-Phase Extraction and Gas Chromatography / Mass Spectrometry

  • Hong, Joo-Yeon;Jung, Ok-Sang;Ryoo, Jae-Jeong;Hong, Jong-Ki
    • Bulletin of the Korean Chemical Society
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    • v.30 no.1
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    • pp.61-66
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    • 2009
  • An analytical method based on solid-phase extraction and gas chromatography / mass spectrometry has been developed for measurement of acaricides (amitraz, bromopropylate, coumaphos, cymiazole, and tetradifon) in honey sample. In the stability test of acaricides in honey, amitraz underwent a rapid degradation into 2,4-dimethylaniline (DMA), 2,4-dimethylphenylformamide (DMPF), and N-(2,4-dimethylphenyl)-N'-methylformamidine (DMPMF), whileas other acaricides were found to be stable even for over three months. Extraction of five acaricides from 5g of honey sample was carried out by liquid-liquid extraction using 20mL of ethylacetate. For purification, Florisil-SPE cartridge with elution of 5mL of n-hexane/ acetone (55:45, v/v) was found to remove interferences effectively. Quantification was performed using gas chromatography / mass spectrometry in the selected ion monitoring mode. Spiking experiments were carried out to determine the recovery, precision, and limits of detection (LODs) of the method. The overall recovery values from honey spiked at 0.02 and 0.20 ${\mu}g/g$ levels, respectively, were found to be greater than 75% for all acaricides. The method detection limits for acaricides were ranged from 0.1 to 3 ppb. The developed method in this study was applied for the monitoring of acaricides in honey products collected from urban markets in Korea.

A Study on North Korea's Cyber Attacks and Countermeasures (북한의 사이버공격과 대응방안에 관한 연구)

  • Chung, Min Kyung;Lim, Jong In;Kwon, Hun Yeong
    • Journal of Information Technology Services
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    • v.15 no.1
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    • pp.67-79
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    • 2016
  • This study aims to present the necessary elements that should be part of South Korea's National Defense Strategy against the recent North Korean cyber-attacks. The elements proposed in this study also reflect the recent trend of cyber-attack incidents that are happening in the Unites States and other countries and have been classified into the three levels of cyber incidents: cyberwarfare, cyberterrorism and cybercrime. As such, the elements proposed are presented in accordance with this classification system. In order to properly take into account the recent trend of cyber-attacks perpetrated by North Korea, this paper analyzed the characteristics of recent North Korean cyber-attacks as well as the countermeasures and responses of South Korea. Moreover, by making use of case studies of cyber-attack incidents by foreign nations that threaten national security, the response measures at a national level can be deduced and applied as in this study. Thus, the authors of this study hope that the newly proposed elements here within will help to strengthen the level of Korea's cyber security against foreign attacks, specifically that of North Korea such as the KHNP hacking incidents and so on. It is hoped that further damage such as leakage of confidential information, invasion of privacy and physical intimidation can be mitigated.

Application and Optimization of the IsoButoxycarbonyl Derivatization method to the Analysis of Trace Level Phenols in Environmental Samples (환경시료로부터 미량 페놀류의 분석을 위한 isoButoxycarbonyl 유도체화 분석방법 적용 및 최적화)

  • Kim, Hyub;Hong, Jong-Ki;Kim, Yong-Hwa;Kim, Kyoung-Rae
    • Environmental Analysis Health and Toxicology
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    • v.17 no.1
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    • pp.37-51
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    • 2002
  • Eleven phenols including two chlorophenols, eight alkylphenols and bisphenol A were derivatized with isobutylchloroformate to form their isobutoxycarbonyl derivatives. Standard phenol mixture was concentrated for the isobutoxycarbonyl (isoBOC) derivatization and analysed by gas chromatography/mass spectrometry (GC/MS). The recoveries of the derivatization method of alkylphenols, chlorophenols, and bisphenol A were calculated by gas chromatography/mass spectrometry-selected ion monitoring mode using two work-up methods for comparison; shaking and heating method. The linear detector responses were obtained in the concentration range of 5∼400 ng, with correlation coefficients varying from 0.9755∼0.9981. Recoveries of the alkylphenols, chlorophenols, and bisphenol A were determined by gas chromatography/mass spectrometry-selected ion monitoring mode using two work-up methods for comparison ; the US-EPA method and the isoBOC derivatization method, Eleven phenols in water samples were extracted with dichloromethane and then concentrated. Also, solid-phase extraction (SPE) with XAD-4 and subsequent conversion to isobutoxycarbonyl derivatives for sensitive analysis with the selected ion-monitoring (SIM) mode. The recoveries were 85.1∼109.9% and 90.3∼126.6% for the US-EPA method and the isoBOC.

Review on the Analytical Methods and Ambient Concentrations of Organic Nitrogenous Compounds in the Atmosphere (대기 유기질소화합물의 분석방법 및 농도)

  • Choi, Na Rae;Kim, Yong Pyo
    • Journal of Korean Society for Atmospheric Environment
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    • v.34 no.1
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    • pp.120-143
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    • 2018
  • The analytical methods and their ambient levels of organic nitrogenous compounds such as nitrosamines, nitramines (nitroamines), imines, amides and nitro-polycyclic aromatic hydrocarbons (nitro-PAHs) in the atmosphere are summarized and discussed. Sampling for the analysis of organic nitrogenous compounds was mostly conducted using high volume air sampler. The direct liquid extraction (DLE) using sonification and the pressurized liquid extraction (PLE) using the accelerated solvent extraction (ASE) have been frequently employed for the extraction of organic nitrogenous compounds in the atmospheric samples. After extraction, clean-up via filtration and the solid phase extraction (SPE) and concentrations using nitrogen and rotary evaporator have been generally conducted but in some studies the clean-up and concentration steps have been omitted to prevent the loss of analyte and improve the recovery rate of the analytical procedure. Instrumental analysis was mainly carried out using gas chromatography (GC) or the high performance liquid chromatography (HPLC) coupled with the single quadrupole mass spectrometer or tandem mass spectrometer in the electron ionization (EI), positive chemical ionization (PCI) and negative chemical ionization (NCI) mode and analysis sensitivity of nitrosamines and nitramines were higher in NCI mode. Desirable sampling and analysis methods for analyzing particulate organic nitrogenous compounds are suggested.