• Title/Summary/Keyword: GC-FID analysis

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Sampling and Analytical Method for Linear Carbonates using GC/FID (GC/FID를 이용한 사슬형 카보네이트 3종의 측정·분석방법)

  • Miyeon Jang;Gwangyong Yi
    • Journal of Korean Society of Occupational and Environmental Hygiene
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    • v.33 no.4
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    • pp.455-463
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    • 2023
  • Objectives: The aim of this study was to develop an air sampling and analytical method for estimating worker exposure to linear carbonate solvents and to evaluate the method. Methods: The target substances were three linear carbonates: DMC, DEC, EMC. GC/FID was used for sample analysis. Laboratory experiments were conducted to determine desorption solvents and sample capacity, and to evaluate storage stability, accuracy, and precision. Results: Coconut Shell Charcoal (CSC, 100/50 mg) was used as the air sampling media, and a desorption solvent of 5% methanol/95% dichloromethane was selected. Recommended sampling capacities were 1~11 ℓ for DMC, 1~18 ℓ for DEC, and 1~24 ℓ for EMC. The stability of three linear carbonates was demonstrated over 30 days in a refrigerator (4℃). Detection limits were determined as follows: DMC 0.26 ㎍/sample, DEC 0.24 ㎍/sample, and EMC 0.25 ㎍/sample. The total coefficient of variation was calculated as DMC 0.064, DEC 0.079, and EMC 0.07. Conclusions: This sampling and analysis method is suitable for estimating personal exposure to linear carbonates in the workplace.

Evaluation of Methodology for the Measurement of VOCs in the Air by Adsorbent Sampling and Thermal Desorption with GC Analysis (흡착포집 및 열탈착/GC 분석에 의한 공기 중 휘발성 유기화합물의 측정방법론 평가)

  • 백성옥;황승만;박상곤;전선주;김병주;허귀석
    • Journal of Korean Society for Atmospheric Environment
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    • v.15 no.2
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    • pp.121-138
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    • 1999
  • This study was carried out to evaluate the performance of a sampling and analytical methodology for the measurement of selected volatile organic compounds (VOCs) in the ambient air. VOCs were determined by the adsorbent tube sampling and automatic thermal desorption coupled with GC/FID and GC/MSD analysis. Target analytes were aromatic VOCs, including BTEX, 1,3,5-and 1,2,4,-trimethylbenzenes(TMBs), and naphthalene. The methodology was investigatedwith a wide range of performance criteria such as repeatability, linearity, lower detection limits, collection efficiency, thermal conditioning, breakthrough volume and calibration methods using internal and external standards. standards. Stability of samples collected on adsorbent tubes during storage was also investigated. In addition, the sampling and analytical method developed during this study was applied to real samples duplicately collected in various indoor and outdoor environments. Precisions for the duplicate samples and distributed volume samples appeared to be well comparable with the performance criteria recommended by USEPA TO-17. The audit accuracy was estimated by inter-lab comparison of both duplicate samples and standard materials between the two independent labs. The overall precision and accuracy of the method were estimated to be within 30% for major aromatic VOCs such as BTEX. This study demonstrated that the adsorbent sampling and thermal desorption method can be reliably applied for the measurement of BTEX in ppb levels frequently occurred in common indoor and ambient environments.

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Comparison of Sampling and Analysis Methods for Volatile Organic Compounds in Ambient Air (대기중 휘발성 유기화합물의 채취 및 분석 방법 비교)

  • 나광삼;김용표
    • Journal of Korean Society for Atmospheric Environment
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    • v.14 no.5
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    • pp.507-518
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    • 1998
  • A field comparison study was carried out to quantify differences among various sampling and analytical methods for volatile organic compounds (VOCs) at a site in Vlsan in June 1997. Air sampling containers (SUMMA canisters) were used by the Korea Institute of Science and Technology (KIST) and adsorption tubes (carbotrap) were used by Yeungnam University (YN Univ.) for sampling ambient air. Duplicate samples obtained by KIST were analyzed by KIST with a GC-MS system for aromatics and halogenated hydrocarbons and by Atm AA with a GC -FID system for C2∼C9 hydrocarbons, respectively. The adsorption tube samples were analyzed by YN Univ. with a GC-FID system for aromatics. VOC levels for the duplicate canister sampls analyzed by KIST and Atm AA were in good agreement. Concentrations of aromatics by the adsroption tube method were generally higher than those by the canister sampling method by factor of 1.5 to 2.0. Differences between the two sampling methods were discussed.

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Determination of Liquid Paraffins in Foods by Using GC-FID (GC-FID를 이용한 식품 중 유동파라핀 함량 분석)

  • Park, Se-Jong;Choi, Jae-Chun;Lim, Ho-Soo;Jang, Su-Jin;Kim, So-Hee;Kim, Meehye
    • Korean Journal of Food Science and Technology
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    • v.45 no.5
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    • pp.545-549
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    • 2013
  • Liquid paraffin is a mixture of heavier alkanes derived from petroleum. It can be used as a lubricant in processing machinery, as a coating agent, or as a releasing agent. The purpose of this study was to analyze liquid paraffins in foods by using a gas chromatography-flame ionized detector (GC-FID). Liquid paraffin was extracted from the food samples using n-hexane. Non-polar aromatic or olefinic co-extractives were removed by alkaline permanganate oxidation followed by clean up on an aluminium oxide SPE cartridge before the GC-FID analysis. The results of recovery tests were 91.5-103.2%. Based on this optimized method, we investigated the amount of liquid paraffin in various food samples purchased from domestic markets. The levels of liquid paraffin in bread were $95.5{\pm}156.0$ mg/kg (0.008%), those in capsules were $40.2{\pm}54.5$ mg/kg (0.001%), and those in dried fruits and vegetables were $3.0{\pm}18.1$ mg/kg (0.0001%). No liquid paraffin was detected in fresh fruits and vegetables. We propose that our method can be used to monitor and detect liquid paraffin in foods for food safety management.

Qualitative, Quantitative Analysis and Chiral Characterization of the Essential Oils of Juniperus phoenicea L. and Juniperus oxycedrus L.

  • Dahmane, Dahmane;Dahmane, Fahima Abdellatif;Dob, Tahar;Chelghoum, Chaabane
    • Natural Product Sciences
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    • v.26 no.1
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    • pp.97-107
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    • 2020
  • Isolation of oils from leaves of Juniperus phoenicea and Juniperus oxycedrus was obtained by steam distillation extraction method. The compositions of essential oils (EOs) were studied by means of GC-MS and GC-FID, using the internal standard method and relative response factors. Around ninety eight compounds were determined in total, representing 98.25 g/100 g of EO of J. phoenicea and 98.48 g/100 g of EO of J. oxycedrus, respectively. The volatile leaf oils were dominated by the terpenic hydrocarbon fractions (79.87 g/100 g) and (61.27 g/100 g) characterized by high contents of α-pinene (64.6 g/100 g) and (54.0 g/100 g) in J. phoenicea and J. oxycedrus, respectively, as the main component. Also, the enantiomeric distribution of α-pinene, sabinene, camphene, δ-3-carene, β-pinene, limonene, linalool, terpinen-4-ol, bornyl acetate, and borneol in both oils is presented for the first time.

Gas Chromatographic Analysis of TDI, MDI and HDI Using 2-Chlorobenzyl Alcohol and 2,4-Dichlorobenzyl Alcohol Derivatives (2-클로로벤질 알코올 및 2,4-디클로로벤질 알코올 유도체를 이용한 TDI, MDI 및 HDI의 가스크로마토그래피 분석)

  • Yun, Ju-Song;Park, Jun-Ho;Lee, Kang-Myoung;Choi, Hong-Soon;Cho, Young-Bong;Koh, Sang-Baek;Cha, Bong-Suk
    • Journal of Korean Society of Occupational and Environmental Hygiene
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    • v.16 no.3
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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.

Purity Assessment of Organic Reference Materials with a Mass Balance Method: A Case Study of Endosulfan-II

  • Kim, Seung-Hyun;Lee, Joonhee;Ahn, Seonghee;Song, Young-Sin;Kim, Dong-Kyum;Kim, Byungjoo
    • Bulletin of the Korean Chemical Society
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    • v.34 no.2
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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.

Simultaneous analysis method of BTEX and TPH in soil (토양중 BTEX와 TPH의 동시분석법에 관한 연구)

  • 신호상;박치후
    • Proceedings of the Korean Society of Soil and Groundwater Environment Conference
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    • 2000.05a
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    • pp.3-8
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    • 2000
  • A simple and rapid simultaneous analysis method of BTEX and TPH in soil was developed. 5g of soil sample were mixed with sodium sulfate and then extracted with 10 mL of mixture of acetone and dichloromethane (1:1). Extraction was performed for 10 min in sonicator and analysis was with GC-FID. The detection limits of BTEX and TPH was 0.8 and 10 mg/kg, respectively. The analytical recoveries were >90% for all BTEX and TPH. Low boiling point fuels and high boiling point fuels are consistently reproduced within RSD 7%. The analysis results show very simple and rapid quantitation of BTEX and TPH in soil sample with low RSD.

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The Determination of Ethyl Isocyanate and Propyl Isocyanate by GC/FID (에틸 이소시아네이트와 프로필 이소시아네이트의 GC/FID 분석)

  • Lee, Eun-Jung;Yoo, Chul;Choi, Hong-Soon;Park, Jun-Ho;Yoon, Ju-Song;Cho, Young-Bong
    • Environmental Analysis Health and Toxicology
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    • v.15 no.1_2
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    • pp.53-59
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    • 2000
  • The purpose of this study is the development of the simple and precise determination method of ethyl isocyanate (EIC) and propyl isocyanate (PIC) through derivatization using secondary aliphatic amines by gas chromatography with flame ionization detector. The urea derivatives are quantitatively and simultaneously derived from EIC and PIC with secondary aliphatic amines such as dipropylamine, dibutylamine. and dipentylamine in methylene chloride, and confirmed by thin layer chromatography and gas chromatography with mass selective detector. For GC/FID, according to the increasing carbon atom of the amines, the retention time and peak area of the urea derivatives are increased. The instrumental detection limits for EIC and PIC were about 23.3∼34.8 $\mu\textrm{g}$ and 21.6∼28.9 $\mu\textrm{g}$, respectively.

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