• Title/Summary/Keyword: GC/MS/SIM

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Liquefaction Characteristics of Polyethylene-Polypropylene Mixture by Pyrolysis at Low Temperature (Polyethylene-Polypropylene 혼합물의 저온 열분해에 의한 액화특성)

  • Cho, Sung-Hyun;Choi, Hong-Jun;Na, Byung-Ki;Lee, Bong-Hee
    • Clean Technology
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    • v.15 no.2
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    • pp.109-115
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    • 2009
  • The low temperature pyrolysis of polyethylene (PE), polypropylene (PP) and polyethylene-polypropylene (PE-PP) mixture in a batch reactor at the atmospheric pressure and $450^{\circ}C$ was carried out to investigate the synergy effect of PE-PP mixture. The pyrolysis time was from 20 to 80 mins. The products formed during pyrolysis were classified into gas, gasoline, kerosene, gas oil and heavy oil according to the petroleum product quality standard of Korea Institute of Petroleum Quality. The analysis of the product oils by GC/MS showed that no new component was detected and no synergy effect was made by mixing of PE and PP. Conversions and yields of PE-PP mixtures were linearly dependent on the mixing ratio of samples.

A Study on Replay Experiments and Thermal Analysis for Autoignition Phenomenon of Shredded Waste Tires (폐타이어 분쇄물의 자연발화현상에 대한 재연실험 및 열분석에 관한 연구)

  • Koh, Jae Sun;Jang, Man Joon
    • Fire Science and Engineering
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    • v.26 no.6
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    • pp.99-108
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    • 2012
  • These days, spontaneous ignition phenomena by oxidizing heat frequently occur in the circumstances of processing and storing waste tires. Therefore, to examine the phenomena, in this work, this researcher conducted the tests of fires of fragmented waste tires (shredded tire), closely investigated components of the fire residual materials collected in the processing and storing place, and analyzed the temperature of the starting of the ignition, weight loss, and heat of reaction. For the study, this researcher conducted fire tests with fragmented waste tires in the range of 2.5 mm to 15 mm, whose heat could be easily accumulated, and performed heat analysis through DSC and TGA, DTA, DTG, and GC/MS to give scientific probability to the possibility of spontaneous ignition. According to the tests, at the 48-hour storage, rapid increase in temperature ($178^{\circ}C$), Graphite phenomenon, smoking were observed. And the result from the DTA and DTG analysis showed that at $166.15^{\circ}C$, the minimum weight loss occurred. And, the result from the test on the waste tire analysis material 1 (Unburnt) through DSC and TGA analysis revealed that at $180^{\circ}C$ or so, thermal decomposition started. As a result, the starting temperature of ignition was considered to be $160^{\circ}C$ to $180^{\circ}C$. And, at $305^{\circ}C$, 10 % of the initial weight of the material reduced, and at $416.12^{\circ}C$, 50 % of the intial weight of the material decreased. The result from the test on oxidation and self-reaction through GC/MS and DSC analysis presented that oxidized components like 1,3 cyclopentnadiene were detected a lot. But according to the result from the heat analysis test on standard materials and fragmented waste tires, their heat value was lower than the basis value so that self-reaction was not found. Therefore, to prevent spontaneous ignition by oxidizing heat of waste tires, it is necessary to convert the conventional process into Cryogenic Process that has no or few heat accumulation at the time of fragmentation. And the current storing method in which broken and fragmented materials are stored into large burlap bags (500 kg) should be changed to the method in which they are stored into small burlap bags in order to prevent heat accumulation.

Evaluation of Testosterone Metabolites/Dehydroepiandrosterone As the Indicators of Testosterone Administration in Horse Doping (경주마 약물검사에서 testosterone 투여 여부표지자로서의 testosterone 대사체들에 대한 dehydroepiandrosterone의 비율 평가)

  • Kim, Jin Young;Choi, Man Ho;Kim, Sung Jean;Kyong, Jin Burm;Chung, Bong Chul
    • Analytical Science and Technology
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    • v.12 no.3
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    • pp.190-195
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    • 1999
  • The metabolism of testosterone ($17{\beta}$-hydroxy-androst-4-en-3-one) was confirmed in horse after a single intramuscular administration of testosterone cypionate (750 mg). Solvent extracts of urine obtained with enzymatic hydrolysis and methanolysis were analyzed by GC/MS after oxime t-butyldimethylsilyl (oxime-TBDMS) derivatization. The structures of four urinary metabolite after testosterone administration in horse were determined based on EI mass spectra and $5{\alpha}$-androstane-$3{\beta}$, $17{\alpha}$-diol and $5{\alpha}$-androstane-$3{\beta}$-ol-17-one as major was confirmed with authentic standard. Also the concentrations of $5{\alpha}$-androstane-$3{\beta}$, $17{\alpha}$-diol, $5{\alpha}$-androstane-$3{\beta}$, $17{\beta}$-diol, dehydroepiandrosterone (DHEA), $5{\alpha}$-androstane-$3{\beta}$-ol-17-one and testosterone were determined in the urine of normal subjects and the urine after administration. The recovery and detection limit in the most drugs were 86.3~94.7% and 1~3 ppb, respectively. Correlation coefficients for calibration were in the range of 0.984~0.999. Excretion profile of testosterone presents the rapid and large increasement up to maximum values at days 5 after administration and the slow regression. The relative ratios of testosterone, its metabolites over DHEA were determined for indication of testosterone administration in horse doping.

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Antioxidative Activity of Extract from Bangah Herb (방아 추출물의 항산화 효과)

  • Jhee, Ok-Hwa;Yang, Cha-Bum
    • Korean Journal of Food Science and Technology
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    • v.28 no.6
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    • pp.1157-1163
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    • 1996
  • Bangah, one of the herbs grown in Korea, was investigated for its antioxidant activity. The ether extracts of bangah herb was separated into neutral, phenolic, acidic and basic fractions and further separated into subfractions. Antioxidative activities were measured by hydrogen donating activity (HDA), peroxide value (POV), thiobarbituric acid (TBA) value and inhibition activity against lipid peroxidation of rat liver microsomes, The subfraction components were identified by GC/MS and NMR. Phenolic, though being very small in quantity, showed higher antioxidant activity at all assay system by hydrogen donating activity. POV, TBA value and inhibition activity against lipid peroxidation of rat liver microsomes. Five subfractions(P-1, P-2, P-3, P-4 and P-5) were fractionated from phenolic fraction of bangah herbs, and subfraction P-2 among them showed strong antioxidant activity on a level with BHT or gallic acid at each assay system. Four compounds (peak I, peak II, peak III and peak IV) were isolated by gas chromatogram of TMS derivatives of subfraction P-2 and thes compounds were confirmed to be phenolic substance having -OH and COOH group. There subfractions (N-1, N-2 and N-3) were fractionated from neutral fraction of bangah herbs, and subfraction N-2 among them showed highest antioxidant activity and inhibition activity against lipid peroxidation of rat liver microsomes. Subfraction N-2 was indentified to be estragole by H-NMR spectroscopy.

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Physicochemical properties of deposited particles on surface of pine leaves as biomarker for air pollution (솔잎가지 표면에 침착된 입자상 물질의 물리화학적 특성 및 대기오염 지표로서의 가능성 고찰)

  • Chung, David;Choi, Jeong-Heui;Lee, Jang-Ho;Lee, Soo-Yong;Lee, Ha-Eun;Park, Ki-Wan;Shim, Kyu-Young;Lee, Jong-Chun
    • Analytical Science and Technology
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    • v.31 no.6
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    • pp.247-258
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    • 2018
  • The purpose of the present study was to investigate whether the degree of air pollution can be evaluated via examination of local plants. Selected sites included two parks in an industrial area, as well as two parks in an urban area. Selected plant samples comprised one-year-old pine shoot leaves. Leaves growing over 2 m from the ground were collected from over 10 pine trees. Leaf surface was analyzed for deposition of 14 trace elements and 16 polycyclic aromatic hydrocarbons (PAHs), including particle size and mass, surface imaging, precipitation-mediated particle removal rate, and concentration. Particle size ranged from 0.4 to $200{\mu}m$, and the volume percentage of particles ${\leq}10$ was 20 %. Deposited particle mass ranged from 0.450-0.825 mg, and precipitation-mediated removal rate ranged from 10.0-27.6 %. Trace element concentration, as measured by ICP/MS after microwave acid digestion, was 18.8-26.3 mg/kg As, 0.08-0.13 mg/kg Be, 0.06-0.08 mg/kg Cd, 4.91-17.8 mg/kg Cr, 5.26-405 mg/kg Cu, 1,930-2,670 mg/kg Fe, 3.03-28.1 mg/kg Pb, 26.9-42.8 mg/kg Mn, 2.66-10.4 mg/kg Ni, 4,560-8,730 mg/kg Al, 2,500-6,120 mg/kg Ba, 5.27-17.8 mg/kg Rb, 40.9-95.3 mg/kg Sr, and 4,030-8,260 mg/kg Zn. Concentration of PAHs, as analyzed by GC/MS/MS after liquid-liquid extraction and purification of deposited particles, ranged from 1.17 to 12.378 mg/kg for ${\Sigma}PAH_{16}$ and from 1.17 to 12.378 mg/kg for ${\Sigma}PAH_7$.

Manufacture Condition of Oleoresin using Citron Peel (유자과피를 이용한 Oleoresin의 제조 조건)

  • Jeong, Jin-Woong;Lee, Young-Chul;Lee, Kyung-Mee;Kim, In-Hwan;Lee, Mie-Soon
    • Korean Journal of Food Science and Technology
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    • v.30 no.1
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    • pp.139-145
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    • 1998
  • This study was performed to provide fundamental data on the optimum manufacture condition of oleoresin using citron peel. Oleoresin was extracted from freeze-dried or hot air dried citron peels using various solvents (hexane, ether, dichloromethane, acetone. and methanol), mixing ratio, extraction temperature, and time. As a result, optimum extraction conditions of oleoresin were: solvent mixing ratio 1:10 (w/v), extraction time 2 hours, and extraction temperature $60^{\circ}C$ when used methanol, and their dichloromethane 1:10 (w/v), 4 hours and $20^{\circ}C$, respectively. At optimum extraction conditions, the yield of oleoresin was shown that 35.79% at hot air drying samples, 32.04% at freeze-dried ones when extracted by methanol, but shown 5.86% and 6.16% when used dichloromethane respectively. The number of volatile components present in citron oleoresin were confirmed as thirty two in methnol extracion method and twenty nine in dichloromethane extraction method by GC and GC/MS, respectively. But, in the kinds and amounts of volatile flavor components, relatively greater numbers of volatiles were identified in freeze-dried sample extracted by dichloromethane compared with other methods. In freeze-dried sample extracted by dichloromethane, volatile components of citron oleoresin predominantly occupied by limonene and ${\gamma}-terpinene$ with about 85%. Other important compounds were shown hydrocarbons. such as ${\alpha}-pinene$, myrcene, terpinolene, ${\beta}-farnesene\;and,\;{\delta}-elemene$, and linalool as alcohols.

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Volatile Flavor Components in Mash of Takju prepared by using Rhizopus japonicus Nuruks (Rhizopus japonicus 누룩으로 담금한 탁주 술덧의 발효 과정 중 휘발성 향기성분)

  • Lee, Taik-Soo;Han, Eun-Hey
    • Korean Journal of Food Science and Technology
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    • v.32 no.3
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    • pp.691-698
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    • 2000
  • Volatile flavor components in the mash of takjus prepared by using Rhizopus japonicus nuruk were identified by using GC and GC-MS. Twenty-four esters, 19 alcohols, 9 acids, 10 aldehydes and 4 others were found in the mash of takju. Thirty nine components including 14 esters and 12 alcohols were detected in the beginning of fermentation. Seventeen components were more detected after second day of fermentation and 66 components were detected after 12 days of fermentation. Thirty eight flavor components including 12 alcohols such as ethanol, 2-methyl-1-propanol and 3-methyl-1-butanol, 14 esters such as ethylacetate, ethylcaprylate and isoamylacetate, 6 aldehydes and 5 acids were usually detected in the fermentation process. Ethanol was predominantly found in the range of 76.2149-92.1155% as a major component by using relative peak area. 3-Methyl-1-butanol, 2-methyl-1-propanol, ethyl caprylate, 2,3-butanediol and benzeneethanol were some of the major volatile components through the fermentation. Peak area of ethylacetate, diethyl succinate, octanoic acid, acetic acid and isobutylaldehyde among the same group were higher than other component depending upon fermentation time.

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Determination of the presence of benzene in vitamin drinks using headspace - solid phase microextraction and gas chromatography - mass spectrometry (Headspace Solid Phase Microextraction-Gas Chromatography/Mass Spectrometry를 이용한 비타민드링크 제품 중 Benzene의 미량분석)

  • Kim, Jong-Hun;Lee, Kyung-Min
    • Analytical Science and Technology
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    • v.20 no.3
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    • pp.237-245
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    • 2007
  • The presence of benzene in 31 products of vitamin drinks purchased from 20 retail outlets was determined using headspace solid phase microextraction (HS-SPME) and gas chromatography-mass spectrometry (GC-MS). The sample (25 ml) was stirred at 1200 rpm for 4 min using a magnetic bar with a $100{\mu}m$ SPME fiber as an adsorbent for benzene which was then desorbed from the fiber for 1 min in the GC injector. Quantitation was achieved using the standard addition method. The limit of detection was determined as 0.56 ng/ml and over a concentration range 0-40 ng/ml the coefficient of correlation was greater than 0.999. The concentration of benzene in the drinks examined was in the range not detectable to 47.35 ng/ml. Benzene was detected in 15 of the drinks with concentration in 5 of them greater than 10 ng/ml which is the limit set for the presence of benzene in the Drinking Water Regulations. The concentrations of benzene in the 5 drinks which exceeded the limit of 10 ng/ml were 16.99, 35.14, 16.03, 47.35 and 14.28 ng/ml respectively.

Determination of trace icing Inhibitors (ether type) in free-floating fuels by gas chromatography-mass spectrometry

  • Shin, Ho-Sang;Ahn, Hye-Sil;Jung, Dong-Gyun
    • Proceedings of the Korean Society of Soil and Groundwater Environment Conference
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    • 2003.04a
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    • pp.196-200
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    • 2003
  • A gas chromatography/mass spectrometric assay method was developed for the simultaneous determination of ethylene glycol monomethyl ether (EGME) and diethylene glycol monomethyl ether (DEGME) in spilled aviation fuels. Ethylene glycol monobutyl ether (EGBE) and ethylene glycol monoethyl ether (EGEE) were used as internal standard and surrogate, respectively. The sample preparation consists of back-extraction with 7 mL of methylene chloride after extraction of 50 mL of fuel with 2 mL of water. The extract was concentrated to dryness and dissolved with 100L of methanol and analyzed by CC-MS (SIM). The peaks had good chromatographic properties by using semi-polar column and the extraction of these compounds from fuel also gave high recoveries of 75 and 85 % with small variations for EGME and DEGME, respectively. Method detection limits were 1.3 ng/mL for EGME and 1.0 ng/mL for DEGME in spilled fuel. The method may be useful for fuel-type differentiation between kerosene and JP-8, which may originate from the storage tank.

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Translocation of Tolclofos-methyl from Ginseng Cultivated Soil to Ginseng (Panax ginseng C. A. Meyer) and Residue Analysis of Various Pesticides in Ginseng and Soil (토양 중 잔류된 Tolclofos-methyl의 인삼(Panax ginseng C. A. Meyer)에 대한 이행 및 잔류 특성)

  • Kim, Ji Yoon;Kim, Hea Na;Saravanan, Manoharan;Heo, Seong Jin;Jeong, Haet Nim;Kim, Jang Eok;Kim, Kwan Rae;Hur, Jang Hyun
    • The Korean Journal of Pesticide Science
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    • v.18 no.3
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    • pp.130-140
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    • 2014
  • Recently, some of the previous studies reported that tolclofos-methyl is still exist in ginseng cultivated soil, even though it is has been banned for ginseng. Therefore, the current study was aimed to examine the levels of absorption and translocation of tolclofos-methyl from ginseng cultivated soil to ginseng root and leaf stem for the period of 1 year. For this study, ginseng plants were transplanted in pots and treated with $5.0mg\;kg^{-1}$ of tolclofos-methyl (50% WP). At the end of each interval periods (every three months) the samples (soil, roots and leaf stems) were collected and analyzed the absorption and translocation levels of tolclofos-methyl using gas chromatography and mass spectrometry (GC-MS). The limit of quantitation of tolclofos-methyl was found to be $0.02mg\;kg^{-1}$ and 70.0~120.0% recovery was obtained with coefficient of variation of less than 10% regardless of sample types. In this study, a considerable amount of translocation of tolclofos-methyl residues were found in soil (4.28 to $0.06mg\;kg^{-1}$), root (7.09 to $1.54mg\;kg^{-1}$) and leaf stem (0.79 to $0.69mg\;kg^{-1}$). The results show that the tolclofos-methyl was absorbted and translocated from ginseng cultivated soil to ginseng root and ginseng leaf stem and found to be decreased time-coursely. Secondly, we were also analyzed soil, root and leaf stems samples from Hongcheon, Cheorwon, Punggi and Geumsan by GC-MS/MS (172 pesticides), LC-MS/MS (74 pesticides). In this study, 43 different pesticides were detected ($0.01{\sim}7.56mg\;kg^{-1}$) in soil, root and leaf stem. Further, tolclofos-methyl was detected 4 times separately in root sample alone which is less ($0.01{\sim}0.05mg\;kg^{-1}$) than their maximum residual limit (MRL) in ginseng. Consequently, the results from both studies indicate the residues of tolclofos-methyl found in ginseng cultivated soil and ginseng ensuring their safety level. Moreover, long-term evaluations are needed in order to protect the soil as well as ginseng free from tolclofos-methyl residues.