• Title/Summary/Keyword: 2중 파장법

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Studies on Analytical Methods for N-Methylcarbamate Residues in Crops by Spectrophotometry and Gas Liquid Chromatography (작물체중(作物體中) N-Methylcarbamate계(系) 농약(農藥)의 잔류분석법(殘留分析法)에 관(關)한 연구(硏究))

  • Oh, Byung-Youl;Jeong, Young-Ho;Park, Young-Sun
    • Korean Journal of Environmental Agriculture
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    • v.1 no.1
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    • pp.14-21
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    • 1982
  • Analytical methods for residues of six N-methylcarbamate insecticides were investigated to compare the minimum detectability, recovery from several crops and feasibility of multiple residue analysis. Those methods studied in this work included spectrophotometry by diazotization and gas chromatography by N-trifluoroacetylation(TFA), pentafluorobenzylether(PFB) and dinitrophenylether (DNP) derivatization. Maximum absorbed wavelength of the diazotized MIPC, XMC, BPMC, propoxur and carbofu ran was around 460 ㎚, while that of carbaryl recorded 510 ㎚. Recovery from brown rice and apple by diazotization method ranged from 80 to 120% and minimum detectable limits were 0.03 to 0.05 ppm in 50 g of the sample. Minimum detectability of PFB derivatives by gas chromatography was superior to TFA and DNP derivatives. DNP derivatives showed the longest retention time among the given derivatives. Recovery from crops by gas chromatographic met hod ranged 74 to 94%, 78 to 93%, and 85 to 99% in brown rice, rice straw and apple, respectively. Limit of detection was 0.01 ppm for TFA, 0.005 ppm for PFB and 0.02 ppm for DNP derivatives in 50 g of the crop samples.

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레이저 유도 형광법(Laser Induced Fluorescence)을 이용한 플라즈마 방전 표시기(Plasma Display Panel)내의 전계 측정에 관한 연구

  • 김정훈;이준학;최영욱;양진호;황기웅
    • Proceedings of the Korean Vacuum Society Conference
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    • 1999.07a
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    • pp.232-232
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    • 1999
  • 교류형 플라즈마 방전 표시기(AC Plasma Display Panel, AC PDP)에 사용되는 플라즈마는 그 부피가 너무 작아서 플라즈마에 변화를 일으키지 않고 그 물성을 관측하기란 쉬운일이 아니다. 그래서 주로 PDP 내의 물성을 관측하는 데 시뮬레이션에 의존하게 된다. 그 물성중에 PDP내의 전계 분포에 대한 정보는 방전의 형성 및 소멸에 대한 많은 단서를 제공하고 있다. 특히 AC PDP의 경우, 유전체에 형성되는 벽적하(wall charge)가 방전의 형성 및 PDP 구동에 중요한 역할을 하는데, 이는 PDP 내의 전계 분포를 살펴봄으로써 대략 예측할 수 있다. 본 연구에서는 시뮬레이션에 의존하지 않고, 직접 레이저 유도 형광법을 이용하여 AC PDP 내의 전계를 측정하였다. 방전 가스인 헬륨(He)의 에너지 준위는 전계의 크기에 따라 에너지 준위가 변화하여, Rydberg(n$\geq$8) 준위가 여러 개의 준위로 나누어지는 현상이 일어나는데, 이를 Stack 효과라고 한다. 따라서 전계의 세기가 커짐에 따라서 각 준위와 준위 사이 값(splitting)이 커지는데, 이를 이용하면 전계를 측정할 수 있다. 즉, 헬륨 원자를 여기시키는 레이저 파장을 변화시키면서 관측되는 레이저 유도 형광 신호를 관측하면, 준위의 splitting을 관측할 수 있다. 본 연구에서는 PDP 내의 전계의 시간적 변화를 관측하였다. 50%, 40kHz의 구형파를 PDP의 두 전극에 가하였을 때, 플라즈마가 켜진 상태뿐만 아니라 플라즈마가 꺼진 후에도 전계에 의한 Splitting 신호가 관측이 되었는데, 전계로 환산하였을 때, 그 값은 대략 수 kV/cm의 값을 갖았는데, 이는 wall charge에 의한 값으로 사료된다.결과로 생각되어진다.플라즈마의 강도값을 입력하여 플라즈마의 radiation을 검출하고, 스퍼터링 공정중 실질적인 in-situ 정보로 이용하였다. PEM을 통하여 In/Sn의 플라즈마 강도변화를 조사하였다. 초기 In/Sn의 플라즈마 강도(intensity)는 강도를 100하여, 산소를 주입한 결과, plasma intensity가 35 줄어들었고, 이때 우수한 ITO 박막을 얻을 수 있었다. Pulsed DC power를 사용하여 아크 현상을 방지하였다. PET 상에 coating 된 ITO 박막의 표면저항과 광투과도는 4-point prove와 spectrophotometer를 이용하여 분석하였고, AES로 박막의 두께에 따른 성분비를 확인하였다. ITO 박막의 광투과도는 산소의 유량과 sputter 된 In/Sn ion의 plasma emission peak에 따라 72%-92%까지 변화하였으며, 저항은 37$\Omega$/$\square$ 이상을 나타내었다. 박막의 Sn/In atomic ratio는 0.12, O/In의 비율은 In2O3의 화학양론적 비율인 1.5보다 작은 1.3을 나타내었다.로 보인다.하면 수평축과 수직축의 분산 장벽의 비에 따라 cluster의 두께비가 달라지는 성장을 볼 수 있었고, 한 축 방향으로의 팔 넓이는 fcc(100) 표면의 경우 동일한 Ed+Ep값에 대응하는 팔 넓이와 거의 동일한 결과가 나타나는 것을 볼 수 있다. 따라서 이러한 비대칭적인 모양을 가지는 성장의 경우도 cluster 밀도, cluster 모양, cluster의 양 축 방향 길이 비, 양 축 방향의 평균 팔 넓이로부터 각 축 방향의 분산 장벽을 얻어낼 수 있을 것으로 보인다. 기대할 수 있는 여러

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Simultaneous Determination and Monitoring of Three Macrolide Antibiotics in Foods by HPLC (Macrolide계 항생물질 동시분석법 확립 및 모니터링)

  • Park, Sang-Ouk;Lee, Sang-Ho;Ahn, Jong-Hoon;Jung, Young-Ji;Kim, Seong-Cheol;Kim, Ji-Yeon;Keum, Eun-Hee;Sung, Ju-Hyun;Kim, Sang-Yub;Jang, Young-Mi;Kang, Chan-Soon
    • Korean Journal of Food Science and Technology
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    • v.42 no.3
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    • pp.287-291
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    • 2010
  • In this study, a simple and rapid pre-treatment method based on liquid extraction was applied for the simultaneous determination of three macrolides (spiramycin, tylosin, and tilmicosin) residues. In these studies, the stock farm products was used as a matrix sample. When the liquid extraction method was compared with the solid phase extraction (SPE) method, the former showed higher recovery percentages and simpler steps than the latter. The macrolids were separated using a reverse-phase C18 ($250\;mm{\times}4.6\;mm$, $5\;{\mu}m$) column and a gradient elution with mobile phases consisting of phosphate buffer (pH 2.5) and acetonitrile. Tylosin and tilmicosin were detected at 288 nm and spiramycin was detected at 232 nm. The average recovery percentage ranged between 83.0-90.2% for samples spiked with the three macrolids at 50 and 100 ng/g The validation results showed that the limit of detection (7 (spiramycin), 12 (tilmiconsin), 12 (tylosin) ng/g)) was under the regulatory tolerances and the linearity from calibration curves was satisfactory for determining the multi-residue of three macrolids in farm products. Monitoring samples were collected at the main cities in Korea as Seoul, Busan, Deajeon, Incheon, Deagu, and Gwangju. Microlide antibiotics were not detected in most samples.

Multiresidue Determination of Tetracyclines in Eggs using Liquid Chromatography with Ultraviolet Detection (액체크로마토그래피를 이용한 계란 중 테트라사이클린계 항생물질의 동시분석법 개발)

  • Lee, Sang-Hee;Shim, You-Sin;Choi, Yoon-Hee;Lee, Beom-Gil;Kim, Hyun-Ju;Shin, Dong-Bin
    • Journal of Food Hygiene and Safety
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    • v.22 no.4
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    • pp.370-374
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    • 2007
  • An analytical method for the simultaneous determination of four tetracycline (oxytetracycline, tetracycline, chlortetracycline, doxycycline) in egg samples was developed and validated using liquid chromatography with ultraviolet detection. Egg samples were extracted by the liquid-liquid extraction based on acetonitrile. The chromatographic separation was achieved on a reverse phase C8 column with gradient elution using a mobile phase of 20 mM oxalic acid (pH 1.5)/acetonitrile. The procedure was validated according to the Food Drugs Administration guideline determining accuracy, precision, and limit of detection. Mean recovery of tetracyclines from spiked egg samples (50, 100, 200, 400, and $800{\mu}g/kg$) were 78.8-109.3%. Linearity in concentration range of $50-800{\mu}g/kg$ was obtained with the correlation coefficient $(r^2)$ of 0.994-0.999. The intra- and inter-day precision (relative standard deviation; RSD) was between 0.3-12.8 and 0.2-11.7%, respectively. Limit of detection (LOD) and limit of quantification (LOQ) for the investigated tetracyclines were 30 and $50{\mu}g/kg$ depending on egg samples, respectively. This method was reliable, sensitive, economical and suitable for routine monitoring of tetracycline residues in dairy egg.

Determination and Survey of Fluoroquinolones Residue in Chicken Muscle by HPLC with Fluorescence Detector (액체크로마토그래피-형광검출기를 이용한 닭고기 중 플루오로퀴놀론계 항균물질 정량분석 및 잔류조사)

  • 박은정;임지흔;이성모
    • Journal of Food Hygiene and Safety
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    • v.19 no.1
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    • pp.12-18
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    • 2004
  • Ofloxacin, norfloxacin, ciprofloxacin, and enrofloxacin in chicken muscle were seperated by liquid extraction and determined with high performance liquid chromatography (HPLC) with fluorescence detector. Analysis was carried out using following conditions; Cl8 column (250${\times}$4.6 mm i.d. 5 ${\mu}{\textrm}{m}$ particle size), mobile phase composed of D.W. (containing 0.4% triethylamine and phospholic acid): methanol : acetonitrile (800:100:100, v/v/v), isocratic pump at a flow rate of 1.0 $m\ell$/min and 50 ${mu}ell$ of injection volume, fluorescence detector with EX278 nm/EM.456 nm. The calibration curves of four fluoroquinolones showed linearity (${\gamma}$$^2$$\geq$0.999) at concenration range of 0.025-0.6 $\mu\textrm{g}$/ml. The recoveries in fortified chicken muscle represented more than 80% with low coefficient of variation (〈10%) for concentration range of four fluoroquinolones. The detection limits for ofloxacin, norfloxacin, ciprofloxacin, and enrofloxacin were 23.5, 3.4, 3.0 and 2.5 ng/g in chicken muscle, respectively. We also monitored fluoroquinolones residue in muscle of chickens (broiler 1:227, Korean native chicken 219, laying chicken 77) using EEC-4-plate screening and HPLC conformation methods. Ten(broiler 5, Korean native chicken 5) out of the fifteen samples which were positively detected by EEC-plate screening method from 1,523 chicken meat were confirmed with ciprofloxacin and enrofloxacin by HPLC. The ranges of residual concentration were 0-0.12 ppm for ciprofloxacin and 0.01-6.79 ppm for enrofloxacin. In conclusion, our method could be applied effectively to determine four fluoroquinolones residues in chicken meat, and further survey for fluoroquinolones residue in chicken meat are needed for more effective control of fluoroquinolones used in livestock.

RETRIEVAL OF VERTICAL OZONE PROFILE USING SATELLITE SOLAR OCCULTATION METHOD AND TESTS OF ITS SCNSITIVITY (태양 엄폐법에 의한 연직 오존 분포 도출과 민감도 실험)

  • 조희구;윤영준;박재형;이광목;요코다타쓰야
    • Journal of Astronomy and Space Sciences
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    • v.15 no.1
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    • pp.119-138
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    • 1998
  • Recently measurements of atmospheric trace gases from satellite are vigorous. So the development of its data processing algorithm is important. In this study, retrievalof vertical ozone profile from the atmospheric transmittance measured by satellite solar occultation method and its sensitivity to temperature and pressure are investigated. The measured transmittance from satellite is assumed to be given by the limb path transmittance simulated using annual averaged Umkehr data for Seoul. The limb path transmittance between wavelengths $9.89{\mu}m$ and $10.2{\mu}m$ is simulated with respect to tangent heights using the ozone data of HALOE SIDS(Hallogen Occultation Experiment Simulated Instrument Data Set) as an initial profile. Other input data such as pressure and temperature are also from HALOE SIDS. Vertical ozone profile is correctly retrieved from the measured transmittance by onion-peeling method from 50km to 11km tangent heights with the vertical resolution of 3km. The bias error of $\pm0.001$ in measured transmittance, the forced error of $\pm3K$ in each layer temperature, and the forced $\pm3%$ error in each layer pressure are assumed for sensitivity tests. These errors are based on the ADEOS/ILAS error limitation. The error in ozone amount ranges from -6.5% to +6.9% due to transmittance error, from -9.5% to +10.5% due to temperature error, and from -5.1% to +5.4% due to pressure error, respectively. The present study suggests that accurate vertical ozone profile can be retrieved from satellite solar occultation method. Accuracy of vertical temperature profile is especially important in the retrieval of vertical ozone profile.

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Hydrothermally Synthesis Nanostructure ZnO Thin Film for Photocatalysis Application (수열합성법으로 합성된 산화아연 나노 구조 박막의 광촉매적 응용)

  • Shinde, N.M.;Nam, Min Sik;Patil, U.M.;Jun, Seong Chan
    • KEPCO Journal on Electric Power and Energy
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    • v.2 no.1
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    • pp.97-101
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    • 2016
  • ZnO has nanostructured material because of unique properties suitable for various applications. Amongst all chemical and physics methods of synthesis of ZnO nanostructure, the hydrothermal method is attractive for its simplicity and environment friendly condition. Nanostructure ZnO thin films have been successfully synthesized on fluorine doped tin oxide (FTO) substrate using hydrothermal method. A possible growth mechanism of the various nanostructures ZnO is discussed in schematics. The prepared materials were characterized by standard analytical techniques, i.e., X-ray diffraction (XRD) and Field-emission scanning electron microscopy (SEM). The XRD study showed that the obtained ZnO nanostructure thin films are in crystalline nature with hexagonal wurtzite phase. The SEM image shows substrate surface covered with nanostructure ZnO nanrod. The UV-vis absorption spectrum of the synthesized nanostructure ZnO shows a strong excitonic absorption band at 365 nm which indicate formation nanostructure ZnO thin film. Photoluminescence spectra illustrated two emission peaks, with the first one at 424 nm due to the band edge emission of ZnO and the second broad peak centered around 500 nm possibly due to oxygen vacancies in nanostructure ZnO. The Raman measurements peaks observed at $325cm^{-1}$, $418cm^{-1}$, $518cm^{-1}$ and $584cm^{-1}$ indicated that nanostrusture ZnO thin film is high crystalline quality. We trust that nanostructure ZnO material can be effectively will be used as a highly active and stable phtocatalysis application.

Development of Analytical Methods for Micro Levels of Naphthalene and TNT in Groundwater by HPLC-FLD and MSD (HPLC-FLD와 MSD를 이용한 지하수 중 나프탈렌 및 TNT의 미량 분석법 개발)

  • Park, Jong-Sung;Oh, Je-Ill;Jeong, Sang-Jo;Choi, Yoon-Dae;Her, Nam-Guk
    • Journal of Soil and Groundwater Environment
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    • v.14 no.6
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    • pp.35-44
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    • 2009
  • Naphthalene and TNT (2,4,6-trinitrotoluene) are defined by U.S. EPA as possible carcinogenic compounds known to have detrimental effects on the aquatic ecosystem and human body. There are, however, few researches on methods of analyzing micro-levels of naphthalene and TNT dissolved in groundwater. This study introduces and evaluates the newly developed analytical methods of measuring naphthalene and TNT in groundwater by using HPLC-FLD (Fluorescence detector) and MSD (Mass detector). The MDL, LOQ and salt effect of these methods, respectively, are compared with those of conventional methods which use HPLC-UV. For the analysis of naphthalene, HPLC-FLD was set in the maxima wavelength (Ex: 270 nM, Em: 330 nM) obtained from 3D-Fluorescence to be compared with HPLC-UV in 266 nM wavelength. The MDL ($0.3\;{\mu}g/L$) and LOQ ($2.0\;{\mu}g/L$) of naphthalene by using HPLC-FLD were approximately 80 times lower than those analyzed by HPLC-UV (MDL: $23.3\;{\mu}g/L$, LOQ: $163.1\;{\mu}g/L$). HPLC-MSD were used in comparison with HPLC-UV in 230 and 254 nM wavelength for the analysis of TNT. The MDL ($0.13\;{\mu}g/L$) and LOQ ($0.88\;{\mu}g/L$) of TNT analyzed by using HPLC-MSD were approximately 130 times lower than those obtained by using HPLC-UV in 230 nM (MDL: $16.8\;{\mu}g/L$, LOQ: $117.5\;{\mu}g/L$). The chromatogram of TNT analyzed by using HPLC-UV in 230 nM displayed elevated baseline as the concentration of ${NO_3}^-$ increases beyond 21 mg/L, while the analysis using HPLC-MSD did not demonstrate any change in baseline in presence of ${NO_3}^-$ of 63.7 mg/L which is 3.5 times higher than average concentration in groundwater. In conclusion, HPLC-FLD and HPLC-MSD may be used as suitable methods for the analysis of naphthalene and TNT in groundwater and drinking water. These methods can be applied to the monitoring of naphthalene and TNT concentration in groundwater or drinking water.

Development of an Analytical Method for Fluxapyroxad Determination in Agricultural Commodities by HPLC-UVD (HPLC-UVD를 이용한 농산물 중 Fluxapyroxad 잔류분석법 개발)

  • Kwon, Ji-Eun;Kim, HeeJung;Do, Jung-Ah;Park, Hyejin;Yoon, Ji-Young;Lee, Ji-Young;Chang, Moon-Ik;Rhee, Gyu-Seek
    • Journal of Food Hygiene and Safety
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    • v.29 no.3
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    • pp.234-240
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    • 2014
  • Fluxapyroxad is classified as carboxamide fungicide that inhibits succinate dehydrogenase in complex II of mitochondrial respiratory chain, which results in inhibition of mycelial growth within the fungus target species. This study was carried out to assure the safety of fluxapyroxad residues in agricultural products by developing an official analytical method. A new, reliable analytical method was developed and validated using High Performance liquid Chromatograph-UV/visible detector (HPLC-UVD) for the determination of fluxapyroxad residues. The fluxapyroxad residues in samples were extracted with acetonitrile, partitioned with dichloromethane, and then purified with silica solid phase extraction (SPE) cartridge. Correlation coefficient($R^2$) of fluxapyroxad standard solution was 0.9999. The method was validated using apple, pear, peanut, pepper, hulled rice, potato, and soybean spiked with fluxapyroxad at 0.05 and 0.5 mg/kg. Average recoveries were 80.6~114.0% with relative standard deviation less than 10%, and limit of detection (LOD) and limit of quantification (LOQ) were 0.01 and 0.05 mg/kg, respectively. All validation parameters were followed with Codex guideline (CAC/GL 40). LC-MS (Liquid Chromatograph-Mass Spectrometer) was also applied to confirm the analytical method. Base on these results, this method was found to be appropriate fluxapyroxad residue determination and can be used as the official method of analysis.

Specific Absorption Coefficients for the Chlorophyll and Suspended Sediment in the Yellow and Mediterranean Sea (황해와 지중해에서의 클로로필 및 부유입자의 비흡광계수 연구)

  • 안유환;문정언
    • Korean Journal of Remote Sensing
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    • v.14 no.4
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    • pp.353-365
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    • 1998
  • Light absorption coefficient per unit mass of particles, i.e., specific absorption coefficient, is important as one of the main parameters in developing algorithms for ocean color remote sensing. Specific absorption coefficient of chlorophyll ($a^*_{ph}$) and suspended sediment ($a^*_{ss}$) were analyzed with a spectrophotometer using the "wet filter technique" and "Kishino method" for the seawater collected in the Yellow and Mediterranean Sea. An improved data-recovery method for the filter technique was also developed using spectrum slopes. This method recovered the baselines of spectrum that were often altered in the original methods. High $a^*_{ph}({lambda})$ values in the oligotrophic Mediterranean Sea and low values in the Yellow Sea were observed, ranging 0.01 to 0.12 $m^2$/mg at the chlorophyll maximum absorption wavelength of 440 nm. The empirical relationship between $a^*_{ph}$(440nm) and chlorophyll concentrations () was found to fit a power function ($a^*_{ph}$=0.039 $^{-0.369}$), which was similar to Bricaud et al. (1995). Absorption specific coefficients for suspended sediment ($a^*_{ss}$) did not show any relationship with concentrations of suspended sediment. However, an average value of $a^*_{ss}$ ranging 0.005 - 0.08 $m^2$/g at 440nm, was comparable to the specific absorption coefficient of soil (loess) measured by Ahn (1990). The morepronounced variability of $a^*_{ss}$ than $a^*_{ph}$ was determined from the variable mixing ratio values between particulate organic matter and mineral. It can also be explained by a wide size-distribution range for SS which were determined by their specific gravity, bottom state, depth and agitation of water mass by wind in the sea surface.