• 제목/요약/키워드: Flame ionization detector

검색결과 115건 처리시간 0.024초

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- (Studies on the Contents of Special Components and Estimation of Purity in Sesame oil -I : Contents of Sesamin and Sterols-)

  • 노일협;이문선
    • Journal of Nutrition and Health
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    • 제16권2호
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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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흡기포트 분사방식의 가솔린 엔진에서 냉시동시 혼합기 형성에 관한 연구 (A Study on Mixture Preparation in a Port Fuel Injection Sl Engine During Engine Starting)

  • 황승환;이종화;민경덕
    • 한국자동차공학회논문집
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    • 제10권4호
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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.

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

  • Park, Hoon;Sohn, Hyun-Joo;Cho, Byung-Goo
    • Journal of Ginseng Research
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    • 제14권3호
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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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연속수증기증류법(SDE)과 동적헤드스페이스법(DHS)에 의한 참기름 중의 향기성분의 분석 (Analysis of Volatiles in Sesame Oil Collected by Simultaneous Distillation/Extraction(SDE) and Dynamic Headspace Sampling (DHS))

  • 하재호
    • 분석과학
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    • 제9권4호
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    • pp.399-405
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    • 1996
  • 참기름 중의 향기성분을 연속수증기증류법(SDE)과 동적헤드스페이스법(DHS)으로 포집하여 GC와 GC-MSD로 동정하였다. SDE로 분석하였을 때 alcohol 6종, aldehyde 6종, ketone 및 acid류 5종, furan 및 phenol류 4종, pyrazine 화합물 12종, pyridine 및 thiazole류 4종, 기타 9종으로 총 46종이 확인되었다. DHS로 분석한 경우 alcohol 3종, aldehyde 6종, ketone, furan 및 phenol류 6종, pyrazine류 12종, pyridine 및 thiazole 4종, 기타 5종으로 모두 36종이 확인되었다. 대부분의 화합물이 SDE법에서 분리된 것이었으나 1-hexanol, pentanal, dimethylsulfide등은 DHS법에 의해서만 분리되었다.

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

  • 이나루;이광용
    • 한국산업보건학회지
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    • 제24권3호
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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.

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

  • 황승환;이종화;박경석
    • 한국자동차공학회논문집
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    • 제7권8호
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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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기체크로마토그래피를 이용한 식이보충제에서 메틸설포닐메탄의 검증된 분석법 개발 (Development of a Validated Determination of Methylsulfonylmethane in Dietary Supplement by Gas Chromatography)

  • 박상욱;이원재
    • KSBB Journal
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    • 제30권4호
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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
    • 분석과학
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    • 제34권5호
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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.

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

  • 노길봉;손현주
    • Journal of Ginseng Research
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    • 제13권2호
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    • pp.183-188
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    • 1989
  • 인삼의 주요 polyacetylens 화합물인 panaxynol, panaxydol 및 panaxytriol의 정량을 위한 GC 분석조건을 확립하였다. 이 때, GC column과 검출기는 SPB-1 fused silica capillary(0.25 mm i, d. $\times$30m, Supelco)와 불꽃이온화검출기(FID)를 사용하였으며 column oven의 온도는 $250^{\circ}C$ 등온이었다. Panaxynol, panaxydol 및 panaxytriol peaks의 retention time은 TMS 유도체화 전의 경우에는 각각 4.2, 5.1 및 6.9분이었으며 TMS유도체화 후에는 각각 4.5, 5.4 및 7.4 분이었다. TMS 유도체화 전의 panaxynol, panaxydol 및 panaxytriol의 정량가능 최소농도는 각각 20, 50 및 100ppm 이었던 데에 비하여, TMS 유도체화 후에는 세 화합물의 정량가능 최소농도가 모두 5ppm의 낮은 수준을 나타내었다. 한편, 홍삼 중의 panaxynol, panaxydol 및 panaxytriol 함량 분석값은 각각 724, 721 과 71$\mu\textrm{g}$/g이었다.

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Purity assignment of 17β-estradiol by mass balance method

  • Lee, Hwa-Shim;Oh, Kwang-Hoon
    • 분석과학
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    • 제30권5호
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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.