• 제목/요약/키워드: Gas Retention Time

검색결과 178건 처리시간 0.032초

Gas Chromatography/Mass Spectrometry에 의한 우육 중의 잔류 Zeranol, Zearalenone 및 그 대사산물들의 동시 분석법에 대한 연구 (A Study on the Simultaneous Determination of Residual Zeranol, Zearalenone and Their Metabolites in Beef by Gas Chromatography/Mass Spectrometry)

  • 이은섭;이용욱
    • 한국식품위생안전성학회지
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    • 제9권1호
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    • pp.1-13
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    • 1994
  • A Simultaneous determination method was improved for the determination and confirmation of zeranol, zearalenone, as well as their isomers and metabolites, in beef. The analytes were extracted from tissue by CH3CN, hydrolyzed enzymatically(for glucuronide conjugates), cleaned up by a strong basic anion exchange resin combined with a liquid/liquid partitioning, derivatized using MSTFA and confirmed, quantified by GC/MS/SIM with a internal standard, zearalane. The results were as follows : (1) all the estrogens were separated on the GC/MS chromatogram under the extraction method and the chromatographic conditions improved, the retention times of zearalane-TMS2, zearalanone-TMS2, zearalenone-TMS2, zeranol-TMS3, taleranol-TMS3, and $\alpha$-zearalenol-TMS3, $\beta$-zearalenol-TMS3, were 18.49, 19.44, 19.63, 19.71, 19.79 and 19.99, 20.08 minutes, respectively. (2) The calibration curves of residual zeranol, zearalenone and their metabolites showed constantly linear(r=0.99) in the range of 5~20 ng. The minimum detection concentration of residual zeranol, zearalenone and their metabolites was 1 ppb. (3) The total average recovery of residual zeranol, zearalenone and their metabolites from spiked beef was 60.2%(CV=29.7%) at the 1 ppb and 63.5%(CV=26.5) at the 2 ppb, 72.9%(CV=18.2%) at the 4 ppb. (4) The preservation method for 6 estrogens was improved for the fast running time(21 min) and MSTFA was utilized for derivatizing 6 estrogens for improvement of recovery, for good resolution, for characteristic mass spectra unlike Jose's method and Tina's method. The utilization of zearalane as internal standard showed good quantification result for zeranol, zearalenone, as well as their isomers and metabolites, in beef.

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Gas chromatography-Thermal Energy Analyzer에 의한 휘발성 니트로소아민과 담배 특유의 니트로소아민들의 동시 분석연구 (Studies on the Simultaneous Determination of VNA and TSNA by GC - TEA)

  • 이문수;지상운;박영수
    • 한국연초학회지
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    • 제15권2호
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    • pp.174-184
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    • 1993
  • This is to investigate the methodology for the simultaneous determination of Wk, mk and TSNA using gas chromatography(GC) in combination with chemiluminescence detector, thermal energy analyzer(TEA) . The simultaneous analysis has been estimated by evaluating tobacco. The TEA was linked to GC equipped with non -polar SPB -5 fused silica capillary column which was introduced into the ceramic pyrolysis tube by the point of 16cm from the end of TEA. Quantification was carried out by internal standardization with WDPA after calibration of retention times and response factors with authentic nitrosoamines. It was demonstrated that WDPA was most preferable as internal standard for the simultaneous analysis. The recoveries of the internal standard were in the range of 83∼96% . Nitrosoamines in this method were detected with determination limit of 0.1ng and was made by a straight line in calibration curve by TEA response. The suitability of nitrosoamines extraction in tobacco leaf was investigated. It was most suitable to extract nitrosoamines from tobacco leaves with 0.01 M NaOH within a period of 8 hours. Thimerosal as an antibacterial agent was added to NaOH solution to prevent artifactual formation. The fractionation and the purification of nitrosoamines form alkaline extracts were conveniently performed using Extrelut multilayer column and dichloromethane. Reproducible and reliable results were obtained for the determination of nitrosamines in a relatively short time compared to previous known method. TSNA contents in burley were about 4 times higher as those in the fluecured tobacco.

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Pilot-scale 회전식 드럼 바이오필터를 이용한 Styrene 제거 (Removal of Gaseous Styrene using a Pilot-Scale Rotating Drum Biotrickling Filter)

  • 황재웅;임지성;장석진;이은열;최차용;박성훈
    • KSBB Journal
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    • 제21권3호
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    • pp.188-193
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    • 2006
  • 본 연구에서는 신 개념의 바이오필터 시스템인 RDBF를 이용하여 기상의 styrene을 제거하고자 하였다. 다양한 운전조건에서 시스템의 성능을 평가하고, 진공흡입을 통해 과다성장 미생물을 제어하고자 하였다. RDBF에서는 sheet 형태의 충진 담체를 사용하므로 영양원 및 공기의 균일한 공급이 가능하였고, 빠른 속도로 균일한 미생물 층을 담체 표면에 형성할 수 있었다. 또한 기-액 접촉면적을 증대 시켜 95% 이상의 안정적이고 높은 styrene 분해 효율과 $125g/m^3{\cdot}hr$의 높은 제거 용량을 가질 수 있게 해주었다. 하지만 우수한 성능은 미생물의 과다성장에 따른 기공의 폐쇄현상 때문에 오래 지속되지 않았고 반응기의 성능과 안정성은 급속히 저하되었다. 이를 해결하기 위해 진공흡입을 통한 미생물 제거를 시도하였으나 제한적인 효과만을 확인하였다. 향후 RDBF 반응기의 상업화를 위해서는 보다 효율적인 미생물 제어 방법이 개발될 필요가 있다.

기상 톨루엔의 생물학적 여과에 관한 실험적 연구 (Experimental Study on the Biofiltration of Toluene Gas)

  • 홍성도;명성운;최석호;김인호;이현재;구본탁
    • KSBB Journal
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    • 제15권5호
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    • pp.469-473
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    • 2000
  • 본 연구는 실험실 규모의 biofilter를 이용하여 공기 중에 혼합되어 있는 대표적인 휘발성 유기화합물인 toluene기체를 제거하는 실험이다. 생물여과실험은 일반적인 조건하에서 오 염된 공기를 바이오필터의 상단으로부터 하단으로 흐르게 하 여 수행하였다. 반웅기 컬럼의 내부는 peat와 calstone (부피 비 5:3) 혼합물로 충진 되었으며, 충진재는 반응기에 채우기 전에 미생물 (Pseudomonas putida type A)과 잘 혼합하였다. 접종된 미생물은 충진 고체충에 고정화되어 생물막을 형성하 게 된다. 바이오필터는 다양한 툴루엔 농도와 유속조건에서 약 90일 이상 운전 되었으며, 최대 제거량은 유입 toluene량 $30 g/m^3hr$에서 $20 g/m^3hr$임을 알 수 있었다. 오염왼 공기는 체류시간 1-2 min에서 제거율이 20-90%끼지 변화하는 것을 보여 주었다 한편 운전중에 발생하는 압력강하는 $1.062 cmH_2O/m$ 정도로서 반응기 전체를 통하여 무시할 수 있을 정도로 낮았다.

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Isocratic 조건하에서 HPLC를 이용한 산업시설 배출가스 중 포름 알데하이드 분석 (An Analytical Method of Formaldehyde in Exhaust Gases from Industrial Facilities using a HPLC under Isocratic Conditions)

  • 김준표;박승식;배민석
    • 한국대기환경학회지
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    • 제34권4호
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    • pp.616-624
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    • 2018
  • In this study, a previous DNPH (2,4-dinitrophenylhydrazine) coupled with high performance liquid chromatography (HPLC) method to measure the concentration of formaldehyde in ambient and source environments has been improved. To improve the disadvantage of the previous HPLC method, an appropriate composition ratio of mobile phase (water: acetonitrile (ACN)) was determined and an isocratic analysis was conducted. Furthermore, limit of detection (LOD), limit of quantitation(LOQ), accuracy, and precision were investigated to verify the reliability of the analytical conditions determined. Finally, samples of exhaust gases from five different industrial facilities were applied to HPLC analytial method proposed to determine their formaldehyde concentrations. The appropriate composition ratio of the mobile phase under the isocratic condition was a mixture of water(40%) and ACN(60%). As the volume fraction of the organic solvent ACN increases, retention time of the formaldehyde peak was reduced. Detection time of formaldehyde peak determined using the proposed isocratic method was reduced from 7 minutes(previous HPLC method) to approximately 3 minutes. LOD, LOQ, accuracy, and precision of the formaldehyde determined using standard solutions were 0.787 ppm, 2.507 ppm, 93.1%, and 0.33%, respectively, all of which are within their recommended ranges. Average concentrations of the formaldehyde in five exhaust gases ranged from 0.054 ppm to 1.159 ppm. The lowest concentration (0.054 ppm) was found at samples from waste gas incinerator in a bisphenol-A manufacturing plant. The highest was observed at samples from the absorption process in manufacturing facilities of chemicals including formaldehyde and hexamine. The analytical time of the formaldehyde in ambient air can be shortened by using the isocratic analytical method under appropriate mobile phase conditions.

염소계 VOCs의 UV 광분해 연구: 제거율 및 부산물 (UV Photodegradation of Chlorinated VOCs: Removal Efficiency and Products)

  • 강인선
    • 한국대기환경학회지
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    • 제33권2호
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    • pp.87-96
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    • 2017
  • In this study, 4 gases containing typical chlorinated volatile organic compounds (VOCs) were treated by ultraviolet (UV) irradiation. The typical chlorinated VOCs are dichloromethane (DCM), trichloromethane (TCM), carbon tetrachloride (CTC) and trichloroethylene (TCE). The removal efficiency (RE) and the products of chlorinated VOCs by UV irradiation are investigated. At this time, 2 types of background gas (air and nitrogen) were used to figure out the RE by photooxidation and photolysis. The specification of UV-lamp used in this study was low-pressure mercury lamp emitting wavelength of 185~254 nm. The experimental conditions were set as initial VOC concentration of $180{\pm}10ppm$, empty bed retention time (EBRT) of 53 s, temperature of $23{\pm}2^{\circ}C$ and relative humidity of $65{\pm}5%$. In the photolysis condition with nitrogen ($N_2$) as background gas, the averaged RE of the 4 types of chlorinated VOCs was about 24% higher than that with photooxidation; and the REs of VOCs except CTC were confirmed as >99%. The composition of off-gases after UV photooxidation in air was investigated and several intermediates from DCM, TCM and TCE were detected by GC/MS. Among them, phosgene which is a toxics was detected as an intermediate of TCM. In addition, the concentration of carbon dioxide ($CO_2$) in the off-gases was measured to calculate the mineralization rate (MR). With the photooxidation, TCE showed the highest RE (>99%) while MR was the lowest (17%); and the MR of DCM was the highest (86%). In addition, particulate matters (PM) in the off-gases was also detected and high concentrated $PM_{10}$ ($21,580{\mu}g{\cdot}m^{-3}$) and $PM_{2.5}$ ($6,346{\mu}g{\cdot}m^{-3}$) were detected in TCE off-gas. More than 99% of the chlorinated VOCs could be removed using UV254-185 nm lamp, while it is necessary to conduct further studies on the production and treatment of secondary pollutants.

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

  • 오도석;김성화;고은아;전형우
    • 대한화학회지
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    • 제63권4호
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    • pp.246-252
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    • 2019
  • GC-OTC/FID(Gas chromatography-Open Tubular Column/Flame Ionization Detector) 계에서 극성 용매(Alcohols)를 분리 하기 위하여 DMSO(Dimethyl sulfoxide)를 사용하였다. 이 계에서는 극성 용매들 보다 DMSO가 늦게 용출이 된다. 이런 계에서 크로마토그래픽 인자인 조정된 머무름 시간($t_R^{\prime}=t_R-t_O$)과 용량 인자{$k^{\prime}=(t_R-t_O)/t_O$} 및 분리 인자{${\alpha}=(t_{R2}-t_O)/(t_{R1}-t_O)$}를 구하기 위하여 불감시간($t_O$)이 필요하다. 그러나 이런 계에서 $t_O$ 를 구하기 위한 보고가 현재까지 된 바가 없기 때문에, 본 연구에서는 $t_O$ 를 구하는 방법을 개발하고자 하였다. $t_O$ 를 계산하기 위하여 DMSO의 머무름 시간($DMSO\;t_R$)을 상용로그로 전환하였다($f(x)={\log}\;t_{R(DMSO)}{\rightarrow}t_O$, $t_O={\log}$ 9.551=0.980). 개발된 방법의 적합 여부를 확인하기 위하여 $CH_4$$t_R$${\ln}\;t_{R(DMSO)}$${\log}\;t_{R(DMSO)}$와 비교하였다. 세 가지 방법 중 $CH_4\;t_R$${\ln}\;t_{R(DMSO)}$는 k' 과 ${\alpha}$를 계산하는데 적합하지 않았다. 본 연구에서 개발한 방법인 ${\log}\;t_{R(DMSO)}$는 일반적인 기준인 k'(1${\alpha}(1<{\alpha}<2)$를 만족하였다. 본 연구에서 개발한 계산방법은 쉽고 편리하기 때문에, 이와 유사한 계에서도 활용될 것으로 기대된다.

토양(土壤)과 채소중(菜蔬中) Phorate(0,0-diethyl S-ethylthiomethyl phosphorithioate)와 그 대사산물(代謝産物)들의 GLC분석(分析) (Determination of Phorate (0,0-diethyl S-ethylthiomethyl phosphorithioate) and its Metabolites in Soil and Vegetables by GLC)

  • 홍종욱;이해근
    • Applied Biological Chemistry
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    • 제26권2호
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    • pp.104-109
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    • 1983
  • phorate와 그 대사산물(代謝産物)들의 잔류분(殘留分) 분석방법(分析方法)을 확립(確立)코자 10% DC-200+8% Reoplex-400+2% QF-1(2 : 1 : 1, w/w/w) on Gas Chrom Q( $80{\sim}100$ mesh), $1.8m{\times}2mm$ ID, borosilicate glass column인 mixed phase column을 이용(利用), flame photometric detector가 부착(附着)된 gas chromatograph로 조사(調査)하였다. 본(本) mixed phase column은 비록 phorate와 5가지 대사산물(代謝産物)을 동시(同時)에 분리(分離)하지는 못하였으나 column온도(溫度)를 programming$(130{\sim}200^{\circ}C,\;5^{\circ}C/min)$함으로써 phoratoxon sulfoxide를 제외(除外)한 5가지 화합물(化合物)의 분리(分離)가 가능(可能)하였다(phoratoxon sulfoxide는 phoratoxon과 중첩되었음). 또는 검출감도(檢出感度)도 매우 높아 $0.05{\sim}3.15ng$범위(範圍)이었다. 한편 토양(土壤)과 채소(菜蔬)에 처리(處理)한 phorate와 그 대사산물(代謝産物)들을 methanol-acetone-benzene(1 : 1 : 1, v/v/v)으로 Soxhlet장치(裝置)에서 12시간(12時間) 추출(抽出)한 후 benzene으로 이들 화합물(化合物)을 분리(分離)한 결과(結果) 90%이상(以上)의 높은 회수율(回收率)(phoratoxon은 약(約) 84%)을 얻었다. 따라서 본(本) mixed phase column은 분리(分離)와 감도면(感度面)에서 그 성능(性能)이 우수(優秀)하여 phorate의 분해(分解)와 대사(代謝)의 연구(硏究)에 효율적(效率的)으로 이용될 수 있을 것이다.

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W 도핑된 ZnO 박막을 이용한 저항 변화 메모리 특성 연구

  • 박소연;송민영;홍석만;김희동;안호명;김태근
    • 한국진공학회:학술대회논문집
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    • 한국진공학회 2013년도 제44회 동계 정기학술대회 초록집
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    • pp.410-410
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    • 2013
  • Next-generation nonvolatile memory (NVM) has attracted increasing attention about emerging NVMs such as ferroelectric random access memory, phase-change random access memory, magnetic random access memory and resistance random access memory (RRAM). Previous studies have demonstrated that RRAM is promising because of its excellent properties, including simple structure, high speed and high density integration. Many research groups have reported a lot of metal oxides as resistive materials like TiO2, NiO, SrTiO3 and ZnO [1]. Among them, the ZnO-based film is one of the most promising materials for RRAM because of its good switching characteristics, reliability and high transparency [2]. However, in many studies about ZnO-based RRAMs, there was a problem to get lower current level for reducing the operating power dissipation and improving the device reliability such an endurance and an retention time of memory devices. Thus in this paper, we investigated that highly reproducible bipolar resistive switching characteristics of W doped ZnO RRAM device and it showed low resistive switching current level and large ON/OFF ratio. This may be caused by the interdiffusion of the W atoms in the ZnO film, whch serves as dopants, and leakage current would rise resulting in the lowering of current level [3]. In this work, a ZnO film and W doped ZnO film were fabricated on a Si substrate using RF magnetron sputtering from ZnO and W targets at room temperature with Ar gas ambient, and compared their current levels. Compared with the conventional ZnO-based RRAM, the W doped ZnO ReRAM device shows the reduction of reset current from ~$10^{-6}$ A to ~$10^{-9}$ A and large ON/OFF ratio of ~$10^3$ along with self-rectifying characteristic as shown in Fig. 1. In addition, we observed good endurance of $10^3$ times and retention time of $10^4$ s in the W doped ZnO ReRAM device. With this advantageous characteristics, W doped ZnO thin film device is a promising candidates for CMOS compatible and high-density RRAM devices.

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리기다소나무재(材)의 유기용매(有機溶媒) 추출물(抽出物)과 그 tall oil 간의 조성(組成)의 차이(差異) (Difference of the Chemical Compositions Between Petroleum Ether Extract and its Tall Oil in Pitch Pine, Pinus Rigida Mill)

  • 고상운;안운영
    • Journal of the Korean Wood Science and Technology
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    • 제16권2호
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    • pp.79-89
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    • 1988
  • 본(本) 실험(實驗)은 리기다소나무(Pinus rigida Mill)를 petroleum ether로 추출(抽出)한 추출액(抽出被)과 흑액(黑液)으로부터 얻은 tall oil과의 조성(組成)의 변화(變化)를 조사(調査)하기 위하여 실시(實施)하였다. 생재(生材)의 유기용매(有機溶媒) 추출액(抽出液)과 tall oil 을 DEAE-Sephadex 칼럼과 aluminum oxide 칼럼을 사용하여 수지산(樹脂酸)과 지방산(脂肪酸)으로 분리(分離)한 후 이를 개스크로마토 그래프로 분석(分析)하였다. 본(本) 실험(實驗)에서 얻는 결과(結果)는 다음과 같다. 생재(生材)의 유기용매(有機溶媒) 추출액(抽出液힘)과 tail oil은 주로 수지산(樹脂酸)으로 구성(構成)되어 있고 특히 abietic-type acide의 함량(含量)이 매우 높게 나타났으며, tall oil의 조성(組成)은 생재(生材)의 유기용매(有機溶媒) 추출물(抽出物)에 비(比)해 지방산(脂肪酸)의 함량(含量)이 증가(增加)한 반면 수지산(樹脂酸)은 감소(減少)하였고, 증해시(蒸解時) 고온(高溫)과 증해약품(蒸解藥品)에 의하여 불포화(不飽和) 지방산(脂肪酸)의 이중결합(二重結合) 위치(位置)의 변화(變化) 및 이성질화(異性質化)에 의하여 미확인(未確認) 물질(物質)의 양(量)이 증가(增加)하였다.

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