• Title/Summary/Keyword: 컬럼시험

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The Effects of Physico-chemical Properties of soils on PCBs Analysis (토양의 이화학적 특성이 PCBs 분석에 미치는 영향)

  • Kim, Tae-Seung;Shin, Sun-Kyoung;Chang, Jun-Young
    • Analytical Science and Technology
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    • v.16 no.1
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    • pp.48-58
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    • 2003
  • The effects of physico-chemical properties of soils on PCBs analysis in Korea was studied Three kinds of extraction solvents(toluene, acetone:hexane, dichloromethane) was selected to apply three different soils. The silicagel, florisil and alumina column cleanup also performed to compare the elution patterns, and three different methods (EPA, Japan, Proposed method in this study) of 62 PCBs also compared the individual peaks recoveries. The solvent average recovery was surveyed the order of toluene, acetone:hexane, dichloromethane as 77.94%, 58.59%, 54.20% for soil A, 53.65%, 80.32%, 68.27% for soil B and 44.52%, 60.35%, 56.36% for soil C, respectively. The average recovery was depended on the soil characters. The highest recoveries of each soil were obtained the toluene for soil A, acetone:hexane for soil B and C. However, the coplanar PCBs was obtained the highest recovery with dichloromethane. Thus, to select the solvent for the analysis of PCBs in solid, the selected compounds have to consider to get good result. The silicagel, florisil, alumina I and alumina II column cleanup process were surveyed the range of 38.73%~98.26%, and the higher chlorinated compounds was obtained the lower recovery compared to the low chlorinated compounds, generally. This results are also consistent with the coplanar PCBs isomers. The compared results of three different countries were obtained the 37.15% for USA, 45.92% for Japan and 44.46% for proposed method in this study.

HPLC를 이용한 축육(Pork Muscle)내의 Dihydrostreptomycin 검출법

  • Choe, Ji-Hyeon;Han, Eun-Yeong;Park, Jin-Gwan;Lee, Su-Yeon;Choe, Dong-Mi;Sin, Ho-Cheol;Lee, Chi-Ho
    • Proceedings of the Korean Society for Food Science of Animal Resources Conference
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    • 2005.10a
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    • pp.196-203
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    • 2005
  • 축산식품 고기내의 잔류항생물질을 신속하고 간편하고 정확하게 분석하기 위한 시험법 개발 을 목적으로 하였다. 축산식품내의 일반적인 잔류항생물질에 대한 지금까지의 분석법으로는 Bioassay법, TLC법, ELISA법, GC법 및 HPLC법 등이 있지만 Streptomycin/Dihydro streptomycin, Neomycin에 대한 HPLC법은 거의 확립되어 있지 않은 실정이다. 우리나라의 공인 검사법으로는 Bioassay법 및 HPLC법 등이 있지만 그러나 지금까지의 방법으로는 검출감도가 낮은 것이 큰 문제점으로 되어 왔다. 본 연구에서는 DST에 대한 HPLC법에 대한 보고한 P. Edder 방법 중에 clean-up과정 및 이동상 조건을 대폭 수정하여 DST의 분리 및 검출감도를 낮추려고 시도하였다. 본 연구에 사용된 유도체화 장치 Post-Column Derivatization Instrument PCX 5100 (Pickering Laboratories, Inc.)의 컬럼온도는 $40^{\circ}C$, 오븐온도 $55^{\circ}C$, reagent 유속 0.6ml/min mobile phase 유속 0.8ml/min으로 검출기는 형광검출기를 이용하여 DST 검출에 대해 만족할 만한 결과를 얻었다. 이때의 분석소요시간은 약 15분이었다. 표준시료 DST의 검량선은 넓은 농도범위(0.02${\sim}$1.0ppm)에서 양호한 직선성을 나타냈다. 본 시험법에 의한 검출한계는 limit of detection (LOD)은 0.02ppm이었으며, 적어도 고기에서의 MRL이 0.6ppm임을 감안하면 DST를 정량적으로 정도 좋게 측정할 수 있다는 것을 확인했다. 상기의 조건하에서 실제시료인 고기에 표준 DST를 1ppm을 spiking한 후 SPE상에서 SCX(Strong cation exchange column)을 통한 clean-up과정을 거친 후의 DST의 limit of quantification(LOQ)는 약 0.47ppm이었으며, 이에 대한 회수율은 97.7%(n= 8)를 나타냈다. 실제 codex에서 권장한 고기의 MRL이 0.6ppm인 점을 감안하면 codex 권고치에 도달할 수 있는 것으로 판단되었다. 따라서 본 연구에서 개발된 시험법은 지금까지 국내적으로 DST에 대한 시험법이 확립되어 있지 않은 것으로 이와 아울러 간편한 parallux와 병용해 DST에 대한 정량 및 정성 분석을 유도체화 장치 및 형광검출기를 이용해 잔류항생물질 DST에 대한 분석시험법의 개발이 가능하다고 여겨진다.

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HPLC를 이용한 우유 중에 잔류 항생물질(Streptomycin)의 정량 분석

  • Byeon, Jang-Won;Park, Hwan-Seok;Hong, Go-Eun;Hong, Mu-Gi;Park, Gwan-Ha;Lee, Chi-Ho
    • Proceedings of the Korean Society for Food Science of Animal Resources Conference
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    • 2005.10a
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    • pp.310-316
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    • 2005
  • 축산식품(우유)내의 잔류항생물질을 신속하고 간편하고 정확하게 분석하기 위한 시험법 개발을 목적으로 하였다. 축산식품내의 일반적인 잔류항생물질에 대한 지금까지의 분석법으로는 Bioassay법, TLC법, ELISA법, GC법 및 HPLC법 등이 있지만 Streptomycin/dihydrostreptomycin, neomycin에 대한 HPLC법은 거의 확립되어 있지 않은 실정이다. 우리나라의 공인 검사법으로는 Bioassay법 및 HPLC법등이 있지만 그러나 지금까지의 방법으로는 검출감도가 낮은 것이 큰 문제점으로 되어 왔다. 본 연구에서는 STP에 대한 HPLC법에 대한 보고한 Edder 방법 중에 clean-up 과정 및 이동상 조건을 대폭 수정하여 STP의 분리 및 검출감도를 낮추려고 시도하였다. 본 연구에 사용된 유도체화 장치 Post-Column Derivatization Instrument PCX 5100 (Pickering La-boratories, Inc.)의 컬럼 온도는 $40^{\circ}C$, 오븐온도 $55^{\circ}C$, 유도체화 용매 유속 0.6ml/min 이동상 유속 0.8ml/min으로 검출기는 형광검출기를 이용하여 STP 검출에 대해 만족할 만한 결과를 얻었다. 이때의 분석소요시간은 약 15분이었다. 표준시료 STP의 검량선은 넓은 농도범위(0.02${\sim}$1.0ppm)에서 양호한 직선성을 나타냈다. 본 시험법에 의한 검출한계는 limit of detection(LOD)은 0.02ppm이었으며, 적어도 우유에서의 MRL이 0.6ppm임을 감안하면 STP를 정량적으로 정도 좋게 측정할 수 있다는 것을 확인했다. 상기의 조건하에서 실제시료인 우유에 표준 STP를 0.5ppm을 spiking한 후 SPE상에서 SCX(Strong cation exchange column)을 통한 clean-up과정을 거친 후의 STP의 limit of quantification(LOQ)는 약 0.44ppm이었으며, 이에 대한 회수율은 89.7${\pm}$2.3%(n=6)를 나타냈다. 실제 CODEX에서 권장한 우유의 MRL이 0.6ppm인 점을 감안하면 CODEX권고치에 도달할 수 있는 것으로 판단되었다. 따라서 본 연구에서 개발 된 시험법은 지금까지 국내적으로 STP에 대한 시험법이 확립되어 있지 않은 것으로 이와 아울러 간편한 parallux와 병용해 STP에 대한 정량 및 정성 분석을 유도체화 장치 및 형광검출기를 이용해 잔류항생물질 STP에 대한 분석시험법을 개발하였다.

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Desalinization of marine soil by the application of straw and lime (개흙의 제염에 미치는 볏짚, 석회의 병용효과)

  • Oh, Wang-Keun
    • Korean Journal of Soil Science and Fertilizer
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    • v.24 no.1
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    • pp.35-40
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    • 1991
  • A laboratory column experiment was conducted to learn the desalinization effect of rice straw, fresh or predecayed in limed marine soil, compared with gypsum. One third of Ca equivalent to indigenous Na plus Mg of the soil was applied to the top 10g out of 80g of total column soil, mixing one half of it to the top soil and the rest spreading on the surface. 1. Pre-decaying of rice straw in limed marine soil promoted the permeability of column soil. but showed a less effectiveness in desalinization of sodium than lime alone or lime plus fresh rice straw treatemenents. 2. Gypsum and calcium carbonate treatments without rice straw fixed Mg in the limed top soil and washed it down disolving more from the layer immediatly be low the treated top soil But the treatment of calcium carbonate and rice straw both together washed out Mg more from lower layers than the upper's, showing only physical desalinization. 3. The desalinization of Na was also severe in the layer immediately below the $CaSO_4$ treated top soil, leauing more Na ilo the top soil, which seemed to be attributed to the peptisation of the top soil and retard peptisation of desalinization when washed the soil applying not enough amount or non of gypsum.

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Validation of urinary N-methylacetamide reference material for proficiency test (숙련도시험을 위한 소변 중 N-메틸아세트아미드 표준시료 검증)

  • Lee, Mi-Young
    • Analytical Science and Technology
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    • v.27 no.6
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    • pp.339-346
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    • 2014
  • The author assessed the availability of urine reference material for proficiency test provided for laboratories in occupational health. N-methylacetamide is the biomarker of exposure to N,N-dimethyl acetamide, which was used as the substitute for hepatotoxic N,N-dimethylformamide (DMF). N-methylacetamide (NMAC) urine samples of 3 different levels covering the 0.2~2 times of the exposure limit were tested. Stability test up to 180 days (0, 7, 30, 60, 180 days) at 4 different temperatures (-60, -20, 5, $25^{\circ}C$) and homogeneity test were performed for these samples. New analytical condition by GC/MSD using SIM mode (m/z 58, 59) and DB-624 column was investigated for better selectivity, sensitivity and resolution. Urinary NMAC samples showed good homogeneity for 3 levels. These samples also showed good stability up to 180 days. The data of stability and homogeneity of urinary DMAC confirmed the basis of including this item into Korean proficiency test for occupational health laboratories since 2008.

The Evaluation on the Environmental Effect of Coal-Ash and Phosphogypsum as the Evapotranspiration Final Cover Material (증발산 원리를 이용한 매립장 최종 복토공법의 복토재로서 석탄재와 인산석고의 환경적 영향 평가)

  • Yu, Chan;Yang, Kee-Sok
    • Journal of the Korean GEO-environmental Society
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    • v.6 no.1
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    • pp.15-21
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    • 2005
  • In this study, the utilization of coal-ash and phosphogypsum was considered as the evapotranspiration final landfill cover(ET cover) material. Cover material considered was the mixture of the weathered granite soil, coal-ash and phosphogypsum and so we sequentially performed the leaching test, column test and field model test to investigate the environmental effects of mixtures of coal-ash and phosphogypsum. In the leaching test, all materials had lower heavy metal concentration than the regulated threshold values. The column test and the review of related regulations were carried out to determine the optimum mixing ratio(OMR) and OMR was soil(4):coal-ash(1): phosphogypsum(1) on the volume base, which was applied to field model test. Field model tests were continued from February to June, 2004 in the soil box that was constructed with cement block. It was verified that coal-ash and phospogypsum mixed with soil was safe environmentally and the mixture of both wastes could improve the water retention capacity of cover materials.

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An Equation for the Prediction of Material Function of Super Soft Clay (초연약 점토의 구성관계 산정식)

  • Kang, Myoung-Chan;Lee, Song
    • Journal of the Korean Geotechnical Society
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    • v.19 no.1
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    • pp.221-228
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    • 2003
  • In land reclamation construction using marine clay, a measure of material function, that is, the relation between void ratio-effective stress and permeability, is very important aspect for the prediction of self-weight consolidation behavior. But reclaimed ground has very high water content, so there are many difficulties in the laboratory test for measuring material function. For this reason, some researches are carried out using slurry cconsolidometr to measure material function. In this study, material function was measured using slurry consolidometer, and to overcome the shortcoming of researches using slurry cosolidometer, an equation for the prediction of material function was proposed on the basis of column test's parameter. Material function was determined through low stress consolidation test and permeability test, and it also was calculated with the equation using column test parameter. The continuity of material function could be confirmed through these tests. Material function is easily determined with the equation proposed in this study, and can be used for the prediction of self-weight consolidation behavior.

The Purification Characteristics of Reactive Soil-Bentonite Landfill Liner (혼합반응 차수재의 오염정화특성)

  • 김학문
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.4 no.4
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    • pp.398-403
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    • 2003
  • The purpose of this paper is to investigate purification characteristic of soil-bentonite landfill liner and to develop a desirable liner system. In order to clarify the purification characteristics, high pressure column tests using soil-bentonite, reactive soil-bentonite and reactive bentomat were carried out in the presence of water and leachate. The test results indicated that the significant amount of NH$_3$-N, Pb and Cu was removed through the reactive soil-bentonite liner system.

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Fate of Nitrogen and Phosphorous in Hydroponic Waste Solution Applied to the Upland Soils (시설하우스 폐양액의 토양 처리에 따른 질소 및 인의 이동)

  • Yang, Jae-E.;Park, Chang-Jin;Yoo, Kyung-Yoal;Kim, Kyung-Hee;Ok, Yong-Sik
    • Korean Journal of Environmental Agriculture
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    • v.24 no.2
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    • pp.132-138
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    • 2005
  • Objective of this research was to evaluate the fate of nitrogen and phosphorous in hydroponic waste solution from the plastic film house cultivation applied to the upland soil by column leaching and field experiment. The pH and EC of leachate were decreased by the reaction with the upland soil in the column leaching experiment. The EC and concentrations of $H^+,\;K^+,\;and\;{NH_4}^+$ of leachate were decreased as the column length (soil depth) was increased. But these were increased as the amounts of the hydroponic waste solution were increased field experiment growing red pepper (Capsicum annum L.) to monitor the nutrients movement using ion exchange resin capsule demonstrated that the nutrient concentration of soil solution was increased in the orders of $PO_4-P. Nitrate concentration of resin capsule inserted into the soil was relatively higher than other nutrients $(NH_4-N\;and\;PO_4-P)$ at the 45 cm of soil depth. The overall results demonstrated that the hydroponic waste solution could be recycled as plant nutrients to enhance fertility of soils. But nitrate leaching was a major factor for safe use of the hydroponic waste solution in soil.

Development of Rapid Analysis Method for Pesticide Residues by GC-MS/MS (GC-MS/MS를 이용한 잔류농약 신속검사법 개발)

  • Choi, Yong-Hoon;Nam, Hye-Seon;Hong, Hye-Mi;Lee, Jin-Ha;Chae, Kab-Ryong;Lee, Jong-Ok;Kim, Hee-Yun;Yoon, Sang-Hyeon
    • The Korean Journal of Pesticide Science
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    • v.9 no.4
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    • pp.292-302
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    • 2005
  • Condition of Ion-Trap gas chromatography-mass spectrometry (GC-MS) for rapid screening of 206-pesticides residues in agricultural foodstuffs was optimized. As applying a wide-bore column (10 m${\times}$0.53 mm, DF 0.25 um) connected with a fused silica restrictor (0.6 m${\times}$0.1 mm), a significant retention time reduction was obtained. Additionally, the shape of peaks was sharper and higher than classical GC's and GC-MS's, which allowed lower detection limits. To easily manage many spectral data, both of Electron Ionization(EI) and Chemical Ionization(CI) techniques were adopted in screening procedure. At the following steps, MS-MS technique were used to confirm screened analytes in complicated matrices.