• Title/Summary/Keyword: 기체 크로마토그래피-질량분석기

Search Result 33, Processing Time 0.025 seconds

Analytical Determination of Alkylphenols, Chlorophenols and Bisphenol A in Biota Samples using Gas Chromatography/Mass Spectrometry (기체 크로마토그래피/질량분석기를 이용한 생물시료 중 알킬 페놀류, 클로로페놀류 및 비스페놀 A의 분석법)

  • Hong, Jongki;Kim, Hyup;Baek, In-Girl;Kim, Do-Gyun;Seo, Jung-Joo;Seo, Jong-Bok;Chung, Bong-Chul;Pyo, Hee-Soo;Kim, Kyung-Rae;Kim, Yong-Hwa
    • Analytical Science and Technology
    • /
    • v.13 no.4
    • /
    • pp.484-493
    • /
    • 2000
  • The simultaneous analysis of alkylphenols, chlorophenols and bisphenol A in biota samples was performed by gas chromatography-mass spectrometry-selected ion monitoring mode. The phenols were extracted from sample with organic solvent and Forisil and Silica columns for clean-up procedure were compared. Recovery studies were performed at 1-ppm level of phenols added to each biota sample. Their recoveries ranged between 83 and 116% with coefficient of variations of 2.4-11.9%. To improve the detection limits of phenols, trimethylsilyl (TMS) derivatization was applied. The gas chromatographic properties of free phenols and TMS derivatized phenols were also investigated.

  • PDF

Determination of Polybrominated Diphenyl Ethers(PBDEs) in Soil using Gas Chromatography/Isotope Dilution Mass Spectrometry (기체크로마토그래피/동위원소 희석 질량분석법을 이용한 토양 중 폴리브롬화 디페닐에테르의 분석법)

  • Na, Yuncheol;Chang, Yoon-Seok;Kim, Hai-Dong;Hong, Jongki
    • Analytical Science and Technology
    • /
    • v.17 no.1
    • /
    • pp.29-36
    • /
    • 2004
  • An analytical method of polybrominated diphenyl ethers in soil samples by isotope dilution method using gas chromatography/mass spectrometry (GC/MS)-selected ion monitoring (SIM) was described. PBDEs in soil were extracted with soxhlet extractor and then silica and florisil solid phase extraction (SPE) methods as purification of extract were compared. After clean-up, the extractions were analyzed by GC/MS with SIM mode. Quantitation was performed isotope dilution method using four $^{13}C$ isotopically labeled PBDEs as internal standards. This developed method was validated for eight congeners of PBDEs in the concentration range 0.04~4 ng/g in soil and the average recovery of the analytes ranged 30.8~110.8% for florisil and 44.4~110.7% for silica, respectively. The method detection limits of PBDEs were 0.04~0.3 ng/g.

Effects of Temperature on the Coking Characteristics of Kerosene (케로신 연료의 침탄 특성에 대한 온도의 영향)

  • Kim, Min Cheol;Kim, Yeong Jin;Kim, Jeong Soo
    • Journal of the Korean Society of Propulsion Engineers
    • /
    • v.23 no.2
    • /
    • pp.46-52
    • /
    • 2019
  • This research was conducted to analyze the effects of temperature on coking characteristics of kerosene. The kerosene was heated to 600 K, 700 K, and 800 K, and the cooled samples were collected. The used copper tubes were replaced according to the temperature conditions. The liquid and copper specimens were analyzed by gas chromatography-mass spectrometry and scanning electron microscopy equipped with an energy dispersive x-ray spectrometer, respectively. The results of the analysis confirmed that a carbon deposit was formed from the coking of fuel on the inner surface of the copper specimen at a relatively high temperature (800 K) of the copper tube.

Determination of Phthalates in Biota Samples Using Gas Chromatography/Mass Spectrometry (기체크로마토그래피/질량분석법을 이용한 생체시료 중 프탈산 에스텔류의 분석법)

  • Seo, Jung-Ju;Na, Yuncheol;Hong, Jongki
    • Analytical Science and Technology
    • /
    • v.14 no.5
    • /
    • pp.400-409
    • /
    • 2001
  • A method for the analysis of most common phthalate acid esters (9 secies) in biota samples by gas chromatography-mass spectrometry-selected ion monitoring mode is described. Phthalates in biota samples are extracted by organic solvent and purified by Florisil column. Phthalates are easily contaminated during extraction prodedure. Since the extraction and cleanup steps for biota samples generally are more complicate than those for water or sediment samples, we compared with contamination state of each sample work-up step. By applying this developed method, the overall recoveries ranged between 79 - 117% in biota sample which was spiked with standards. For phthalates used in this study, the quantitaive accuracy, elution pattern on Florisil column, and detection limits were also investigated.

  • PDF

Determination of allyl isothiocyanate, capsaicin and dihydrocapsaicin in pungent liquid samples (자극성 액체시료 중 Allyl Isothiocyanate, Capsaicin and Dihydrocapsaicin 정량에 관한 연구)

  • Kim, Sang-Soo;Choi, Jong-Moon
    • Analytical Science and Technology
    • /
    • v.26 no.1
    • /
    • pp.73-79
    • /
    • 2013
  • The allyl isothiocyanate, capsaicin and dihydrocapsaicin as main components in self defense sprays were determined by gas chromatography-mass spectrometer (GC-MS). Although self defense spray was used to protect by myself, a social problem could be caused by the hazard of spray chemical due to use pungent liquid. To identify this, the pH of pungent liquid solutions, solubility to detergents, the existence of other materials and the types and amounts of pungent material in spray chemicals were investigated in this work. Finally, the amounts of allyl isothiocyanate, capsaicin and dihydrocapsaicin as pungent materials in them were determined by GC-MS. The pH of chemicals were about 5.7 as weak acid, the detergents can emulsify them with water well. And they did not contain fluorescent materials and hazard organic solvents. The pungent components in three real samples were only allyl isothiocyanate [47,600 mg/kg (47.6%)] in one sample, and mixtures with capsaicin [228 mg/kg~368 mg/kg (1.14%~1.84%)] and dihydrocapsaicin [224 mg/kg~414 mg/kg (1.12%~2.07%)] in the others, respectively.

Simultaneous determination of aromatic material causing allergic in children's products by Gas Chromatography (어린이 제품 중 가스 크로마토그래피를 이용한 알러지 유발 방향성 물질의 동시분석법)

  • Ko, Kyeong Mok;Rhu, Chan Joo;Kim, Jong Won;Lee, Seok Ki
    • Analytical Science and Technology
    • /
    • v.31 no.1
    • /
    • pp.23-30
    • /
    • 2018
  • Twenty-two allergy-induced aromatics in children were analyzed using a gas chromatography flame ionization detector (GC-FID) and gas chromatography mass spectrometer (GC-MSD). Analytes were extracted using an automatic Soxhlet extractor and centrifuged for 10 min in a fast freezing centrifuge, and the supernatant was transferred into a 2 mL vial and injected in split mode. Under the established conditions, the calibration curve showed linearity with a correlation coefficient of 0.996 or more. A wide range of sensitivity of 6.7 to 1,859,839 depending on the device characteristics and detector used was shown. The detection limit of the device was 0.0032 to $0.0335{\mu}g/mL$, and the maximum detection limit was less than $0.1{\mu}g/mL$. The detection limit of the method ranged from 0.0033 to $0.1161{\mu}g/mL$. In addition, the limit of quantification ranged from 0.0100 to $0.5422{\mu}g/mL$, with a level of precision ranging from 0.21 % to 4.89 % and a degree of accuracy ranging from 89 % to 111 %. The analytical method developed in this study was applied to commercial products.

Comparison of isoButoxycarbonyl derivatives, tert.-butyldimethylsilyl derivatives, with US EPA Method in the sensitivity of Alkylphenols, Chlorophenols, and Bisphenol A Potential field-screening applications of GC/MS-SIM (기체 크로마토그래피/질량분석기를 이용한 field-screening 적용을 위한 알킬페놀류, 클로로페놀류 및 비스페놀 A의 isoBOC 유도체, TBDMS 유도체와 US EPA 방법의 비교)

  • Kim, Hyub;Hong, Jong-Ki;Kim, Yong-Hwa;Kim, Kyoung-Rae
    • Analytical Science and Technology
    • /
    • v.15 no.3
    • /
    • pp.196-213
    • /
    • 2002
  • The alkylphenols, chlorophenols and bisphenol A were determined by gas chromatography/mass spectrometry-selected ion monitoring mode followed by three work-up methods for comparison; EPA method, isoBOC derivatization method and TBDMS derivatization method. Eleven phenols in water samples were extracted with dichloromethane. Also, solid-phase extraction (SPE) with XAD-4 and subsequent conversion to isobutoxycarbonyl derivatives or tert.-butyldimethylsilyl derivatives for sensitive analysis with the selected ion-monitoring (SIM) mode. The recoveries were 85.1~109.9% (EPA method) and 90.3~126.6% (isoBOC derivatization and TBDMS derivatization), respectively. The method detection limit of bisphenol A for SIM were 0.732 ${\mu}g/{\ell}$ (EPA method), 0.002 ${\mu}g/{\ell}$ (isoBOC derivatization) and 0.021 ${\mu}g/{\ell}$ (TBDMS derivatization). The SIM responses were linear with the correlation coefficient varying 0.9755~0.9981 (isoBOC derivatization), and 0.9908~0.9996 (TBDMS derivatization). When these methods were applied to treated wastewater sample from a polyethylene plant, the concentrations of 11 phenols were below the method detection limit.

Determination of Polybrominated Biphenyls in Biota Samples Using Gas Chromatography/Mass Spectrometry (기체크로마토그래피/질량분석법을 이용한 생체시료 중 Polybrominated Biphenyls의 분석법)

  • Hong, Jongki;Baek, In-Girl;Kim, Hyub;Kim, Do-Gyun;Seo, Jung-Joo;Seo, Jong-Bok;Park, Hyun-Mee;Lee, Kang-Bong
    • Analytical Science and Technology
    • /
    • v.13 no.5
    • /
    • pp.666-674
    • /
    • 2000
  • The present study describes an analytical method for the determination of polybrominated biphenyls (PBBs) in biota samples by gas chromatography-mass spectrometry (GC/MS). PBBs are extracted twice from 20 g samples with mixture solvent 40mL acetone and 80mL hexane using ultrasonic agitation for 20 min. Lipids in extracts are degraded by concentrated sulfuric acid and then PBBs are purified with Florisil column. The purified extracts are analyzed by GC/MS-selected ion monitoring mode for the quantitation of PBBs in biota sample. The overall recovery yields of PBBs range between 77 and 111% under these experimental conditions.

  • PDF

Removal of Off-flavor from Laminaria Japonica by Treatment Process of Supercritical Carbon Dioxide (초임계 이산화탄소 처리 공정에 의한 다시마 유래 이취성분 제거)

  • Park, Jung-Nam;Kim, Ryoung-Hee;Woo, Hee-Chul;Chun, Byung-Soo
    • Clean Technology
    • /
    • v.18 no.2
    • /
    • pp.191-199
    • /
    • 2012
  • In order to reduce or remove off-flavor and volatile organic compounds (VOCs) from Laminaria japonica effectively, continuous treatment process by supercritical carbon dioxide (SC-$CO_2$) was applied. After freeze-drying, Laminaria japonica powdered with $710{\mu}m$ was used. Experiments were carried out at temperature range from 35 to $55^{\circ}C$, and pressure range from 10 to 25 MPa for evaluation of SC-$CO_2$ treatment effect. Flow rate of carbon dioxide used in this reseach was constantly fixed at 26.81 g/min. Before and after treatment of SC-$CO_2$, off-flavor and VOCs from Laminaria japonica were analyzed by gas chromatography-mass spectrometry detector (GC-MSD). Total 47 VOCs emitted from Laminaria japonica were identified before treatment of SC-$CO_2$, major components of seaweed smell (ordor) in Laminaria japonica were identified as alcohols, aldehydes, ester and acids, ketone, halogenated compounds and hydrocarbon. Off-flavor and VOCs in all experimental conditions was reduced or removed after SC-$CO_2$ treatment. Among the experimental conditions, the highest removal yield was at 25 MPa and $55^{\circ}C$.