• 한국산업보건학회지
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• 제16권3호
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• pp.222-232
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• 2006

Objectives: The objective of this study was to propose the total isocyanate analytical method which involves derivation of 2,4-toluene diisocyanate(2,4-TDI), 2,6-toluene diisocyanate(2,6-TDI), 4,4'-methylenediphenyl diisocyanate(4,4'-MDI) and 1,6-hexamethylene diisocyanate(1,6-HDI) using 2-chlorobenzyl alcohol(2-CBA) or 2,4-dichlorobenzyl alcohol(2,4-DCBA), and analyzing of hydrolysate of the synthesized urethane with the gas chromatography(GC)/flame ionization detector(FID), GC/pulsed discharge ionization detector-electron capture detector(PD-ECD) and GC/mass selective detector(MSD). Methods: Urethanes were synthesized by reacting 2,4-TDI, 2,6-TDI, 4,4'-MDI and 1,6-HDI to 2-CBA or 2,4-DCBA. Urethanes was verified by TLC, HPLC/UVD and GC/MSD. For field application, the most suitable condition that 2-CBA coated in glass fiber filter removed completely and urethanes were not removed was searched. 2-CBA generated from hydrolysis of urethanes according to hydrolysis conditions. Diisocyanates were collected on field air and analyzed. Results: Urethanes which were white and solid phase synthesized by reacting 2,4-TDI, 2,6-TDI, 4,4'-MDI, 1,6-HDI and 2-CBA or 2,4-DCBA. And urethanes were verified by TLC, HPLC/UVD and GC/MSD. The most suitable conditions to remove 2-CBA coated in glass fiber filter were $87^{\circ}C$ and 20 mmHg and urethanes were not removed under same condition. Hydrolysis yields of urethanes were 99 % to 111 %. 2-CBA, the hydrolysate of urethanes was analyzed by GC/FID, GC/PD-ECD and GC/MSD. Conclusions: Simultaneous analysis of 2,4-TDI, 2,6-TDI, 4,4'-MDI and 1,6-HDI deriving with 2-CBA and 2,4-DCBA, along with a total isocyanate analysis, was feasible with GC/FID, GC/PD-ECD and GC/MSD. This result will be a guide of further study on total isocyanate analysis.

• 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.

• 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.

• 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.

• 한국토양환경학회지
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• 제3권1호
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• pp.3-9
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• 1998

본 연구는 휘발성 유기 화합물로 오염된 가솔린 지역에서 soil-gas의 분석결과로부터 오염도를 유추하는 기법에 대하여 서술 하였다. Soil-gas의 채취방법으로는 펌프를 이용한 1)grab sampling법과 흡착제 trap을 사용한 2)passive sampling법이 있다. Grab sampling법은 특정시간에 특정장소에서의 오염도를 보여주며, 반면에 passive sampling법은 특정위치에서 시간에 따른 오염도의 변화를 보여 준다. Soil-gas의 분석은 1)PID나 FID와 같은 작은 검지기에 의해서 총괄 탄화수소량을 측정할수도 있고 2)기체농도에 따라서 색깔이 변하는 지시약이 채워진 기체검지기 튜브를 사용할수도 있으며 3)여러가지 화합물을 한 번에 분석할수 있는 이동형 GC를 사용할수도 있다. Soil-gas를 이용한 측정법은 매우 값싸며 세밀한 정밀조사를 하기 위한 전단계에서 사용할 수 있는 유용한 방법으로 추천할만하다 하겠다.

• 한국식품영양과학회지
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• 제11권3호
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• pp.35-36
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• 1982

초유 및 성숙유의 지방질 조성을 TLC-FID 방법으로 분석, 정량하였던 바 분리된 지방질 성분 중 triglyceride 수준이 초유에서보다 성숙유에서 유의하게 높았으며, 기타의 지방질 성분들은 초유 및 성숙유간에 유의한 차이가 나타나지 않았다.

• 오토저널
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• 제13권5호
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• pp.89-94
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• 1991

In the quantitative analysis of oxygenated exhaust emissions (unburned methanol, formal- dehyde) from methanol fueled vehicles, the oxygen contained in oxygenated exhaust gases lowers the FID (Flame Ionization Detector) response factor of conventional THC analyzer and leads to erroneous HC reading. For correct measurement of various HCs including oxygenated HCs emitted from FFV(Flexible Fuel Vehicle), first of all, the measurement technique of real HC emissions should be established. GC and HPLC-DNPH measuring methods specified by the EPA are used in this paper to analyze unburned methanol and formaldehyde components in the exhaust emissions. In emission test of FFV, unburned methanol and formaldehyde are emitted mostly during cold transient period, and it is shown that formaldehyde emission level is proportional to engine displacements. In view of the HC emission level, vehicle using M85 has 40% advantage over gasoline-fueled vehicle in OMHCE and has a good potential of a low emission vehicle.

• 한국지하수토양환경학회지:지하수토양환경
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• 제15권1호
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• pp.9-18
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• 2010

In this study, Solid-phase micro-extraction (SPME) with Gas Chromatograph using Flame Ionization Detector (GC/FID) was studied as a possible alternative to liquid-liquid extraction for the analysis of Methyl tert-butyl ether (MTBE) and Tertiary-butyl ether (TBA) in water and an optimization condition of trace analysis of MTBE and TBA using the design of experiment (DOE) was described. The aim of our research was to apply experimental design methodology in the optimization condition of trace analysis of fuel oxygenated compounds in soil-phase microextraction with GC/FID. The reactions of SPME were mathematically described as a function of parameters of Temp ($X_1$), Volume ($X_2$), Time ($X_3$) and Salt ($X_4$) being modeled by the use of the partial factorial designs, which was used for fitting 2nd order response surface models and was alternative to central composite designs. The model predicted agreed with the experimentally observed result ($Y_1$(MTBE, $R^2$ = 0.96, $Y_2$ (TBA, $R^2$ = 0.98)). The estimated ridge of the expected maximum responses and optimal conditions for MTBE and TBA were 278.13 and (Temp ($X_1$) = $48.40^{\circ}C$, Volume ($X_2$) = 73.04 mL, Time ($X_3$) = 11.51 min and Salt ($X_4$) = 12,50 mg/L), and 127.89 and (Temp ($X_1$) = $52.12^{\circ}C$, Volume ($X_2$) = 88.88mL, Time ($X_3$) = 65.40 min and Salt ($X_4$) = 12,50 mg/L), respectively.

• Bulletin of the Korean Chemical Society
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• 제34권2호
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• pp.531-538
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• 2013

A mass balance method established in this laboratory was applied to determine the purity of an endosulfan-II pure substance. Gas chromatography-flame ionization detector (GC-FID) was used to measure organic impurities. Total of 10 structurally related organic impurities were detected by GC-FID in the material. Water content was determined to be 0.187% by Karl-Fischer (K-F) coulometry with an oven-drying method. Non-volatile residual impurities was not detected by Thermal gravimetric analysis (TGA) within the detection limit of 0.04% (0.7 ${\mu}g$ in absolute amount). Residual solvents within the substance were determined to be 0.007% in the Endosulfan-II pure substance by running GC-FID after dissolving it with two solvents. The purity of the endosulfan-II was finally assigned to be ($99.17{\pm}0.14$)%. Details of the mass balance method including interpretation and evaluating uncertainties of results from each individual methods and the finally assayed purity were also described.

• 한국식품위생안전성학회지
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• 제33권6호
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• pp.483-487
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• 2018

본 연구는 저장 중 조랭이떡에 존재하는 자연균총의 생장특성 및 프로피온산 생성능을 조사하여 떡류에서 프로피온산의 천연유래를 입증하고자 한다. 실험은 저장 중 신선한 조랭이떡과 cocktail Propionibacterium을 오염시킨 조랭이떡 두 가지를 약 3개월까지 저장하여 진행하였다. 저장온도와 저장기간에 따른 조랭이떡에서의 프로피온산 생성량을 측정하였으며, 프로피온산 분석은 GC-FID (Gas chromatograph with Frame ionization detector)를 사용하였다. $30^{\circ}C$에 저장한 주정처리하지 않은 신선한 조랭이떡에서는 1주만에 프로피온산이 약 95 mg/L 검출되었고, 4주 후에 약 330 mg/L, 6주 후에 약 850 mg/L, 8주 후에 약 970 mg/L, 12주 후에 약 1,040 mg/L이 검출되었다. Cocktail Propionibacterium에 오염시킨 조랭이떡은 $30^{\circ}C$에서 1주만에 프로피온산이 약 100 mg/L이 검출되었고, 2주 후에 270 mg/L, 4주 후에 약 470 mg/L, 8주 후에 약 660 mg/L이 검출되었다. 본 연구는 조랭이떡에 존재하는 자연균총인 프로피온산 생성균이 조랭이떡 저장 중 프로피온산을 생성하는 것을 증명하였으며, 이러한 떡류 중 천연유래 프로피온산 생성을 예방하기 위해서는 철저한 위생관리와 $20^{\circ}C$이하에서의 보관이 필요한 것으로 판단된다.