• Title/Summary/Keyword: flame ionization detector

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Studies on the Contents of Special Components and Estimation of Purity in Sesame oil -I : Contents of Sesamin and Sterols- (참기름의 특이성분함량(特異成分含量)과 순도결정(純度決定)에 관(關)한 연구(硏究) (제(第) 1 보(報)) -Sesamin 및 관련(關聯)Sterol를 중심(中心)으로-)

  • Ro, Ihl-Hyeob;Lee, Moon-Sun
    • Journal of Nutrition and Health
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    • v.16 no.2
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    • pp.107-114
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    • 1983
  • There has been no specific test available for identifying the sesame oil among common edible oils. As the contents of sesamin and the ratio of sterols allowed the estimation for the genuine sesame oil, the author investigated to establish some instrumental methods for verification of genuine sesame oil and its distribution in the market. The sesame oil was saponified and the sesamin and sterols were isolated from the unsaponiable fraction by Florisil column chromatography. The individual components were determined by gas- chromatography and sesamin standard (purified sesamin) was obtained by silicagel column chromatography. The gas- chromatographic condition using Flame Ionization Detector supported on 10% OV-101 with di-(2-ethylhexyl) sebacate as an internal standard was suitable, and quantitation of sesamin and sterols, including campesterol, stigmasterol and ${\beta}-sitosterol$ was carried out. The results of this study showed that contents of sesamin in genuine sesame oil were 0.3-0.5% and the ratio of stigmasterol to compesterol was 0.3-0.6 and ${\beta}-sitosterol$ to campesterol 3.0-3.8. The 50 samples from the markets in Seoul were composed of 70% genuine sesame oil, and others were mixed with palm oil, rape seed oil and soybean oil.

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A Study on Mixture Preparation in a Port Fuel Injection Sl Engine During Engine Starting (흡기포트 분사방식의 가솔린 엔진에서 냉시동시 혼합기 형성에 관한 연구)

  • 황승환;이종화;민경덕
    • Transactions of the Korean Society of Automotive Engineers
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    • v.10 no.4
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    • pp.15-22
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    • 2002
  • As the emission regulations on the automobiles have been increasingly stringent, precise control of air/fuel ration is one of the most important issues on the gasoline engines. Although many researches have been carried out to identify the fuel transport phenomena in the port fuel injection gasolines, mixture preparation in the cylinder has not been fully understood due to the complexity of fuel film behavior, In this paper, the mixture preparation during cold engine start is studied by using a Fast Response Flame ionization Detector.(FRFID) In order to estimate the transportation of injected fuel from the intake port into cylinder, the wall wetting fuel model was used. The two coefficient($\alpha$,$\beta$) of the wall-wetting fuel model was determined from the measured fuel mass that was inducted into the cylinder at the first cycle after injection cut-in. $\alpha$( ratio of directly inducted fuel mass into cylinder from injected fuel mass) and $\beta$ (ratio of indirectly inducted fuel mass into cylinder from wall wetted fuel film on the wall) was increased with increasing cooling water temperature. To reduce a air/fuel ratio fluctuation during cold engine start, the appropriate fuel injection rate was obtained from the wall wetting fuel model. Result of air/fuel ratio control, air/fuel excursion was reduced.

Isolation of Volatiles from Panax ginseng Root by Vacuum-Distillation with Freeze-Drying (동결건조시 감압증류되는 인삼의 휘발성물질의 분리)

  • Park, Hoon;Sohn, Hyun-Joo;Cho, Byung-Goo
    • Journal of Ginseng Research
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    • v.14 no.3
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    • pp.353-356
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    • 1990
  • The isolation of volatile compounds by vacuum-distillation with freeze-drying was tested 1 with fresh ginseng roots. The roots were frozen at-8$0^{\circ}C$; they were dried at-4$0^{\circ}C$ tinder vacuum(40 tory), for 24 hours; and the ice condensed at the silrface of condenser in the freeze-dryer was thauved at room temperature. The ether extract of the resulting aqueous solution was analyzed by gas chromatography (GC) equipped with a flame ionization detector (FID) or a nitrogen-phosphorils detecto(NPD) and by gas : chromatography/mass spectrometry(GC/MS). More than forty peaks were observed in the CG(FID) profile. and more than ten peaks were observed in the GC(NPD) profile. Among them, thirteen components 1including one aldehyde, four hydrocarbons, two esters, folly alcohols, and two vyrazines were identified: six components the molesuiar ions of which were m/z, 204 were estimated to be a series of azulene compounds; and the other components unidentified were estimated to have molecular weights of lower than 254. Therefore, the freeze-drying technicue is thought to be usefu1 for the isolation of volatile compounds of such low molecufilar weights from vegetables, fruits and biological fluids as well as fresh ginseng roots under the tested conditions.

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Analysis of Volatiles in Sesame Oil Collected by Simultaneous Distillation/Extraction(SDE) and Dynamic Headspace Sampling (DHS) (연속수증기증류법(SDE)과 동적헤드스페이스법(DHS)에 의한 참기름 중의 향기성분의 분석)

  • Ha, Jaeho
    • Analytical Science and Technology
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    • v.9 no.4
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    • pp.399-405
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    • 1996
  • The flavor compounds of the oil from roasted sesame seeds were collected by simultaneous steam distillation/ extraction(SDE) and dynamic headspace sampling(DHS) and were analyzed using a gas chromatograph equipped with a flame ionization detector and connected into a mass spectrometer. Among the flavor compounds collected by the SDE method, 46 compounds were identified. They consisted of 6 alcohols, 6 aldehydes, 5 ketones or acids, 4 furans or phenols, 12 pyrazines, 4 pyridines or thiazoles, and others. Thirty six compounds were identified by DHS and many of them were the same as those identified by the SDE method. However, some compounds such as 1-hexanol, pentanal, and dimethylsulfide were identified only by the DHS method.

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Research on desorption and stability of benzene, toluene, acetone and n-hexane of activated carbon acquired from domestic market (국내 시판 중인 활성탄을 이용한 벤젠, 톨루엔, 아세톤 및 노말 헥산의 탈착 및 저장성 평가 연구)

  • Lee, Naroo;Yi, Gwangyong
    • Journal of Korean Society of Occupational and Environmental Hygiene
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    • v.24 no.3
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    • pp.353-358
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    • 2014
  • Purpose: This study was conducted to evaluate desorption efficiency and storage stability on activated carbon acquired form domestic market. Materials: Mixture of acetone, benzene, normal hexane and toluene was injected on four types of charcoal 100 mg. After overnight, charcoal was desorbed by carbon disulfide $1m{\ell}$ and analyzed by gas chromatography with flame ionization detector. Results: Desorption efficiency of benzene, normal hexane and toluene in charcoal tubes were 95% ~ 105%. But desorption efficiency of acetone in charcoal tubes was below 75% and different from types of charcoal. The more injected amount of acetone on charcoal showed higher desorption efficiency. Acetone injected on charcoal tubes migrated from front section into back section after 10 days storage at room temperature. Conclusions: Desorption efficiency and storage stability of activated carbon acquired from domestic market was good for benzene, normal hexane and toluene. The activated carbon acquired from domestic market has ability to be used as sampling media.

Estimation of Wall Wetting Fuel at Intake Port and Model Based Prediction A/F in a S.I. Engine (가솔린 엔진에서 액막 연료량 추정 및 이를 이용한 공연비 예측에 관한 연구)

  • 황승환;이종화;박경석
    • Transactions of the Korean Society of Automotive Engineers
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    • v.7 no.8
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    • pp.116-122
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    • 1999
  • According to the stringent exhaust emission regulation, precise control of air fuel ratio is one of the most important issues on gasoline engine. Although many researches have been carried out to identify the fuel transport phenomena in a port fueled gasoline engine, complexity of fuel film behavior in the intake port makes it difficult. The fuel film behavior was investigated recently by using visualization method and these gave us qualitative understanding. The purpose of this study is to estimate of wall wetting fuel in the intake port and the inducted fuel mass was predicted by using wall wetting fuel model . The model coefficient($\alpha$,$\beta$) and fuel film mass on the port wall were determined from measured in-cylinder HC concentration using FRFID after injection off. The fuel film mass was increased, but $\alpha$(ratio of directly inducted fuel mass into cylinder from injected fuel mass) was decreased with increasing load at the same engine speed. $\beta$is nearly constant value(0.8~0.9). when injected fuel mass is varied at 1500rpm , the calculated air fuel ratio using well wetting fuel model was nearly the same as measured by UEGO.

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Development of a Validated Determination of Methylsulfonylmethane in Dietary Supplement by Gas Chromatography (기체크로마토그래피를 이용한 식이보충제에서 메틸설포닐메탄의 검증된 분석법 개발)

  • Park, Sang-Wook;Lee, Wonjae
    • KSBB Journal
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    • v.30 no.4
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    • pp.141-147
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    • 2015
  • The convenient determination of methylsulfonylmethane (MSM) for a commercially available dietary supplement was developed using gas chromatography (GC)-flame ionization detector (FID). Chromatography was performed on a capillary column ($0.32mm\;I.D{\times}30m$, $0.25{\mu}m$) coated with dimethylpolysiloxane using diethylene glycol methyl ether as an internal standard. The performance characteristics of GC were evaluated in terms of selectivity, linearity, precision, accuracy, recovery, limit of detection (LOD) and limit of quantification (LOQ). The calibration curve was highly linear (the coefficient of determination: 0.9979) within the concentration range of $10.0{\sim}800.0{\mu}g/mL$ for MSM. The recoveries for three fortified concentrations were 96.7~97.1%, 96.6~97.3% and 96.8~97.2%, respectively. The LOD and LOQ of the method were $0.29{\mu}g/mL$ and $0.97{\mu}g/mL$, respectively. All obtained results were acceptable according to the guidelines of the Association of Official Analytical Chemists for dietary supplements. Thus, the validated analytical method using the GC-FID system is suitable for the determination of MSM in dietary supplement formulations for quality control.

Development of primary reference gas mixtures of 18 volatile organic compounds in hazardous air pollutants (5 nmol/mol level) and their analytical methods

  • Kang, Ji Hwan;Kim, Yong Doo;Lee, Jinhong;Lee, Sangil
    • Analytical Science and Technology
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    • v.34 no.5
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    • pp.202-211
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    • 2021
  • Volatile organic compounds (VOCs) in hazardous air pollutants (HAPs) have been regulated by the Air Pollution Control Act (1978) and their atmospheric concentrations have been monitored in 39 monitor sites in Korea. However, measurement standards of volatile organic compounds (VOCs) in HAPs at ambient levels have not been established in Korea. Primary reference gas mixtures (measurement standards) at ambient levels are required for accurately monitoring atmospheric VOCs in HAPs and managing their emissions. In this study, primary reference gas mixtures (PRMs) at 5 nmol/mol were developed in order to establish primary national standards of VOCs in HAPs at ambient levels. Primary reference gas mixtures (PRMs) were prepared in pressurized aluminum cylinders with special internal surface treatment using gravimetric method. Analytical methods using gas chromatography-flame ionization detector (GC-FID) coupled with a cryogenic preconcentrator were also developed to verify the consistency of gravimetrically prepared HAP VOCs PRMs. Three different columns installed in the GC-FID were evaluated and compared for the retention times and separation of eighteen target components in a chromatogram. Results show that the HAP VOCs PRMs at 5 nmol/mol were consistent within a relative expanded uncertainty (k=2) of less than 3 % except acrylonitrile (less than 6 %) and the 18 VOCs were stable for 1 year within their associated uncertainties.

Determination of the Concentration of Panaxynol, Panaxydol and Panaxytrio1 by Capillary-GC(FID) (Capillary-GC(FID)에 의한 panaxynol, panaxydol 및 panaxytriol의 정량)

  • 노길봉;손현주
    • Journal of Ginseng Research
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    • v.13 no.2
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    • pp.183-188
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    • 1989
  • A gas chromatographic method was developed for determination of the concentration of three major polyacetylene compounds in ginseng roots---panaxynol, panaxydol and panaxytriol. The column and the detector used were an SPB-1 fused silica capillary (0.2mm i.d.$\times$30m, Supelco) and a flame ionization detector (FID). The column oven temperature was kept at $250^{\circ}C$ isothermally The retention times of panaxynol, panaxydol and panaxytriol peaks were 4.2,5.1 and 6.9 min before TMS-derivatitration and 4.5,5.4 and 7.4 min after TMS-derivatization, respectively. The minimum determinable concentrations of panaxynol, panaxydol and panaxytriol before TMS-derivatiEation were at the 20, 50 and 100 ppm levels, while the concentrations of panaxydol and panaxytriol as well as panaxynol after TMS- derivatisation could be towered to the 5 ppm level. The panaxynol, panaxydol and panaxytriol contents in red ginseng were determined by use of this method after TMS-derivatization : the amounts obtained were 724, 721 and 71$\mu\textrm{g}$/g, respectively.

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Purity assignment of 17β-estradiol by mass balance method

  • Lee, Hwa-Shim;Oh, Kwang-Hoon
    • Analytical Science and Technology
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    • v.30 no.5
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    • pp.226-233
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    • 2017
  • In general, quantitative chemical analysis in various areas including food, the environment, in vitro diagnostics, etc., requires traceability in order to increase the reliability of the measurements. Measurement traceability is a property of an unbroken chain of comparisons relating an instrument's measurements to SI units. Purity analysis is the first process for establishing traceability to SI units in chemical measurements. The purpose of this study is to develop and validate a method of purity assignment for establishing the traceability of $17{\beta}$-estradiol measurements in an in vitro diagnostics field. The establishment of this method is very important as it can be applied to the development of CRM and to the analysis of the purity of other hormones. The method of assignment of the purity of $17{\beta}$-estradiol was developed using the mass balance method and was validated through participation in an International comparison. In the mass balance method, impurities are categorized into four classes as follows: total related structure impurities, water, residual organic solvents, and nonvolatiles/inorganics. In this study, total related structure impurities were characterized by a gas chromatography-flame ionization detector (GC-FID) and a high-performance liquid chromatography-ultraviolet (HPLC-UV) detector, water content was determined by a Karl-Fisher coulometer, and total residual solvents and nonvolatiles/inorganics were checked simultaneously by thermogravimetric analysis (TGA). The purity of the $17{\beta}$-estradiol was 985.6 mg/g and the expanded uncertainty was 2.1 mg/g at 95% confidence. The developed method can be applied to the development of certified reference materials, which play a critical role in traceability.