• Title/Summary/Keyword: 잔류용매

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Studies on Pretreatment for Analysis of Pesticides by Using HPLC and GC (HPLC 및 GC에 의한 농약분석에서 전처리에 대한 연구)

  • Oh, Bo Young;Bae, Jun Hyun;Kang, Jun Gil;Kim, Youn Doo
    • Journal of the Korean Chemical Society
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    • v.43 no.6
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    • pp.663-669
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    • 1999
  • For determination of separated pesticides by using GC and HPLC, liquid-liquid extraction(LLE) and solid phase extraction(SPE) have been carried out to separate and concentrate the organophophorous pesticides such as Diazinon, Fenitrothion, Phosmet, Phosalon and EPN in environmental water samples. ln determination of pesticides by HPLC/UV, SPE has resulted in higher recovery and more precision than LLE, while in determination of pesticides by GC/FPD, vice versa. HPLC/UV after the pretreatment process of sample by solid phase extraction (SPE-HPLC/UV) has suggested the possibility of determination of pesticides ppb level. ln comparison of detection limit, both SPE-HPLC/UV and LLE-GC/FPD are reasonably suitable for analysis of residue pesticides. ln the respect of the rapidity and the solvent required, SPE-HPLC/UV method has proven to be superior to LLE-GC/FPD.

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The Effect of Enzymatic Hydrolysis by Ethanol Organosolv Pretreatment of Corn Stover (에탄올 유기용매 전처리를 이용한 옥수수대의 효소당화)

  • Park, Jang Han;Kim, Tae Huyn;Kim, Jun Seok
    • Korean Chemical Engineering Research
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    • v.54 no.4
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    • pp.448-452
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    • 2016
  • This study is for the effective pretreatment and saccharification of lignocellulosic biomass for a transport fuel receiving attention. The waste water during the pretreatment of biomass is major factor for determining the price of biofuel. Therefore, we conducted high concentration of organosolv pretreatment for decline waste water and reusing the solvent. We confirmed effect of organosolv pretreatment by components analysis and enzymatic hydrolysis of pretreated biomass. The corn stover was used for and 99.5 wt% of ethanol as a organosolv pretreatment. The pretreatment condition was varied 130 to $190^{\circ}C$ during the designated reaction times and the effect of pretreatment was investigated by enzymatic hydrolysis. The highest glucose conversion was more than 68% the pretreatment condition of $190^{\circ}C$ for 70 min or more. The solid remaining was more than 70% and almost of cellulose and hemicellulose were survived.

Studies on the Development of Liquid Chromatographic Methods for Pesticide Residues (II) : The Development of the Analytical Method for Thiocarbamates Herbicides (잔류농약의 액체 크로마토그래피 분석법 개발에 관한 연구 (II) Thiocarbamates 제초제의 잔류농약 분석법 개발)

  • Lee Dai Woon;Choi Yong Wook
    • Journal of the Korean Chemical Society
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    • v.36 no.1
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    • pp.66-74
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    • 1992
  • A method for the multiresidual simultaneous analysis of 11 thiocarbamates was studied using HPLC. Thiocarbamate in Chinese cabbage was analyzed in the order of extraction, partition, and cleanup in their optimum condition. Acetone was chosen as an extracting solvent. As a partitioning solvent, the mixture of 50% methylene chloride and petroleum ether containing extremely small water content showed good recoveries of thiocarbamate from the water layer. Partition efficiency was affected by pH of the water layer; it remained almost constant under the acidic and neutral condition while decreasing under the basic condition. The comparison done in cleanup step showed that the column chromatographic method is superior to the treatment of coagulating reagent. As an absorbent, the mixture of charcoal, magnesia, and celite with the ratio of 1 : 2 : 4 gave better recoveries and also effectively removed chlorophyll. Over the total procedure, the average recoveries for thiocarbamates in Chinese cabbage were 91% at about 2 ppm fortification level within the relative standard deviation of 8%, and the minimum detection limit (MDL) was 2.2${\sim}$9.3 ng.

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Simultaneous analysis of glucocorticoids in bovine muscle and liver by LC-MS/MS (LC-MS/MS를 이용한 소의 근육과 간 중에 잔류하는 glucocorticoids 동시 분석)

  • Shin, Sang-Eun;Cho, Hyun-Woo;Myung, Seung-Woon
    • Analytical Science and Technology
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    • v.23 no.4
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    • pp.405-413
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    • 2010
  • A new method for the simultaneous determination of six glucocorticoids (betamethasone, dexamethasone, prednisone, prednisolone, methylprednisolone, and flumethasone) in meats (bovine muscle, bovine liver) were established. Samples were effectively extracted using C18 cartridge with ethylacetate. Chromatographic separation was achieved using C18 column and negative electrospray ionization mass spectrometry was performed in the Multiple Reaction Monitoring mode for the effective quantitation and qualification of glucocorticoids. Acetonitrile and water (0.1% formic acid) were used as mobile phase and additive for effective electrospray ionization, and gave good chromatographic separation and mass spectrometric sensitivity. The limit of detection (LODs) and the limit of quantitation (LOQs) in spiked blank samples depending on types of matrix and pharmaceuticals were ranged from 0.2 to $1.0\;{\mu}g$/kg and 0.8 to $3.4\;{\mu}g$/kg, respectively. And the recoveries were between 89.5 to 119.6%. The established method showed good recoveries, accuracies, precisions and fast sample preparation and it will be applied to assay of glucocorticoids residues in meat.

Separation of Heavy Metals from Electroplating Waste Water by Solvent Extraction (용매추출법에 의한 광금폐수중 중금속의 분리에 관한 연구)

  • KIM Sung Gyu;LEE Hwa Yeung;OH Jong Kee
    • Resources Recycling
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    • v.12 no.1
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    • pp.25-32
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    • 2003
  • A study on the separation of heavy metals such as iron, copper, zinc and nickel from electroplating waste water has been investigated. The results showed that the PC-88A was more effective extractant for the extraction of zinc and the efficiency of zinc was to be about 100% at pH 2.5. And copper and nickel were extracted about 100% at pH 2 and more than 90% at pH 4~5 with LIX 84, respectively. On the other hand, in the case of solvent extraction of electroplating waste water(Acid-Alkali type) containing heavy metals, the ferric ion was first extracted at pH 2∼2.5 with 20% Naphthenic acid or 10% Versatic acid-10. And then, copper and zinc were extracted at pH 2 with 3% LIX 84 and at pH 2.5∼3 with 20% PC-88A respectively, remaining nickel in the raffinate. In this manner, the heavy metals in electroplating waste water could be effectively separated with solvent extraction method.

A Study on the Neoasozine Residues in Rice Grain by Neutron Activation Method (방사화(放射化) 분석법(分析法)에 의한 미곡(米穀)중 네오아소진 잔류분(殘留分)에 관한 연구(硏究))

  • Kim, Yong-Hwa;Lee, Koon-Ja;Lee, Su-Rae
    • Korean Journal of Food Science and Technology
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    • v.13 no.1
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    • pp.20-24
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    • 1981
  • Residues of neoasozine in rice grain were determined by neutron activation and colorimetric techniques. Twice application of the chemical before flowering did not lead to any increased residue level while 4-times application resulted in significant increase in the residue level up to 0.54-0.75 mg $As_2O_3/kg$. The partition ratio of arsenic residues into polished rice grain and bran was 73 : 27 in 100% polishing while most of the residues in the bran was transferred to oil cake fraction during solvent extraction, reaching up to 2.9 mg $As_2O_3/kg$. The neutron activation technique was advantageous because of its high sensitivity and the smaller sample amounts required for analysis.

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Analytical Method for MCPA Residue in Brown Rice and Rice Straw by HPLC/UVD (HPLC/UVD를 이용한 현미와 볏짚 중 MCPA의 잔류분석방법 확립)

  • Yoo, Ki-Yong;Kang, Dae-Won;Choi, Yong-Hwa;Han, Seong-Soo
    • Korean Journal of Weed Science
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    • v.30 no.4
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    • pp.361-370
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    • 2010
  • This study was carried out to establish the analytical method of MCPA residue in brown rice and rice straw by HPLC/UVD. When MCPA was extracted from sample under the pH 3.6 by adding acetone 200 mL and 1N-HCl 100 mL, the extraction efficiency was high by 87%. And purification efficiency was high by 83% when 5 mL of 1% methanol/acetonitrile was eluated by the florisil Sep-pak cartridge column. From spiking of $0.1{\mu}g\;mL^{-1}$ and $0.25{\mu}g\;mL^{-1}$ of MCPA to control sample, respectively, average recovery rate of MCPA in brown rice was 96.0% and 94.9% and that in rice straw was 92.5% and 88.2%, respectively. Precision of experiment was very high by relative standard deviation of 1.5% to 5.7%. In brown rice and rice straw treated with bentazone+MCPA (11+1.2%) of 30 kg and 60 kg per ha at 30 days after rice transplanting, respectively, maximum residue limit was under $0.05{\mu}g\;mL^{-1}$ of the recommended rate of Korean Food and Drug Administration. From the above results, the analytical procedure of MCPA in plants such as hydrolysis, saponification and derivatization were ommited, and retention time was faster and recovery rate was higher than the existed results of HPLC/UVD. Therefore, these results were greatly improved and seemed to be usefully applied for residue analysis of MCPA in plants.

Effect of alkali chemical compound on paper properties for acidic papers preservation (산성지 보존을 위한 알카리 토금속 화합물이 종이물성에 미치는 영향)

  • 최찬호;신종순;마주희
    • Proceedings of the Korean Printing Society Conference
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    • 2001.06a
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    • pp.45-45
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    • 2001
  • 자료의 보존에 있어서 종이의 열화로 인해 자료의 분석, 열화메커니즘의 해석, 종이의 보존이란 측면 하에서의 관심이 서서히 집중되고 있는 실정이며, 그 중요성도 크게 대두되고 있는 실정이다. 산성지를 중성화하는 화학적시스템, 즉, 탈산성화처리는 알카리계금속(Ca, Mg, Zn, Na)과 유기용매, 수용성용매를 이용하여 이들 약품을 종이내에 침투시켜 중성화(pH 6-8) 함으로써 종이의 주성분인 cellulose를 보다 안정화시키는 방법으로 산을 중화하여 보존성을 향상시킬 수 있는 것이다. 즉, 탈산처리란 화학적으로 종이속에 생기는 산 또는 산을 발생하는 물질을 알칼리물질로 중화하는 것이다. 또한 중화후 알칼리 물질이 종이에 잔류하면 장래에 내부적으로 발생하는 산이나 외부(대기중의 오염물질 등) 로부터 침입하는 산도 중화하여 보존성을 향상시킬 수가 있다. 따라서, 본 연구는 산성초지법에 의해 제조된 용지들의 열화특성과 알카리 토금속을 처리한 후에 알카리도를 상승시킨 용지의 열화특성을 물리·화학적 변화를 통하여 종이의 보존성을 비교 검토·규명함으로써 문(도)서의 보존체계를 마련하고자 하며, 보존과 관련된 기초자료를 얻고자 실시하였다.

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Studies on Simultaneous Analysis of Preservatives by High Pressure Liquid Chromatography in Foods (HPLC를 이용한 식품 보존료의 동시분석에 관한 연구)

  • 김우성;임복규;백종민;박인원;박인원;임연하;지영애;조경종
    • Journal of Food Hygiene and Safety
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    • v.7 no.1
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    • pp.49-52
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    • 1992
  • A Liquid Chromatogaphic Method was applied to analyze the following nine preservatives used for foods simultaneously; propionic acid, sorbic acid, benzoic acid, dehydroacetic acid, ethyl p-hydroxy benzoate, propyl p-hydroxy benzoate, i-butyl p-hydroxy benzoate, butyl p-hydroxy benzoate, ethyl salycilate. A cosmosil $5C_{I8}$ was used and 1% phosphoric acid-acetonitrile (60 : 40) was used as the mobile phase. Pretreatment of the food sample with steam distillation improved the resolution of peaks at 220 nm.

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Effects of In-Situ flushing on the Bioremediation of Soil Contaminated with Endosulfan (In-Situ Flushing기법이 Endosulfan으로 오염된 토양의 생물학적 처리에 미치는 영향)

  • 전민하;최상일
    • Journal of Soil and Groundwater Environment
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    • v.6 no.2
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    • pp.39-47
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    • 2001
  • According to a series of batch-scale washing tests, SDS+$POE_5$ and $POE_5$+$POE_14$ were determined for the applicable mixed surfactants. Because SDS+$POE_5$ showed slightly negative effects on the microbes in the toxicity tests, $POE_5$+$POE_14$((1:1) 1%) was chosen for this study. In the in-situ flushing experiments, the removal rate of endosulfan was 67% for the injection rate of 1.5L/min/$\textrm{km}^2$. And when methanol and ethanol were added as cosolvent, 75% and 81% removal efficiencies were achieved, respectively. In the tests of bioremediation after the application of in-situ flushing, the removal rates of contaminated soils having 13mg/kg dry soil and 3mg/kg dry soil as initial concentrations were 86% and 81%, respectively. There were no significant degradation after 24 hours. The major rate-limiting factor for the biodegradation of endosulfan might be the mass transfer from soil phase to liquid phase after 24 hours. With the addition of surfactant, 89% removal was achieved after 120 hours. Because the surfactant improved the mass transfer rate, the biodegradation of endosulfan was enhanced. When surfactant and cosolvent were added together, the adaptation period of microorganisms to the surfactant became longer and the removal rates were 84% and 83% for methanol and ethanol, respectively.

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