• Title/Summary/Keyword: dynamic headspace/GC-MS

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Semiquantitative Dynamic Headspace GC-MS Analysis for Organic Compounds Outgassed from FAB Materials of Air Shower (에어샤워부품의 용출 가스 중 유기화합물의 반 정량적 Headspace GC-MS 분석)

  • Park, Hyun-Mee;Baig, Soung-Woo;Kim, Young-Man;Lee, Kang-Bong
    • Analytical Science and Technology
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    • v.13 no.4
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    • pp.412-422
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    • 2000
  • The polymeric FAB materials of air shower used in clean room of wafer industry have been outgassed with the dynamic headspace (ca.$100^{\circ}C$) for half an hour, and analyzed using GC-MS. The air in the clean room running air shower was sampled using sorbent tube method, and the organic compounds adsorbed in the sorbent tube were extracted using Soxhlet extraction method, and analyzed using GC-MS. The analytical results from FAB materials of air shower (electric over current relay, acryl plate. polycarbonate window, filter, fan housing, steel galvanized cold plate and canvas buffer) indicated that most of chemicals were originated from polymer fragments of FAB materials. Their analytical results have been compared with those from the air of clean room running air shower. These comparative results could lead to identify whether the sources of trace organic contaminants in clean room air are originated from the polymeric FAB material of air shower.

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Characterization of Fennel Flavors by Solid Phase Trapping-Solvent Extraction and Gas Chromatography-Mass Spectrometry

  • Shin, Yeon-Jae;Jung, Mi-Jin;Kim, Nam-Sun;Kim, Kun;Lee, Dong-Sun
    • Bulletin of the Korean Chemical Society
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    • v.28 no.12
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    • pp.2389-2395
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    • 2007
  • Headspace solid phase trapping solvent extraction (HS-SPTE) and GC-MS was applied for the characterization of volatile flavors from fennel, anise seed, star-anise, dill seed, fennel bean, and Ricard aperitif liquor. Tenax was used for HS-SPTE adsorption material. Recoveries, precision, linear dynamic ranges, and the limit of detection in the analytical method were validated. There were some similarities and distinct differences between fennel-like samples. The Korean and the Chinese fennels contained trans-anethole, (+)-limonene, anisealdehyde, methyl chavicol as major components. The volatile aroma components from star anise were characterised by rich trans-anethole, (+)-limonene, methyl chavicol, and anisaldehyde. Additionally, principal component analysis (PCA) has been used for characterizing or classifying eight different fennel-like samples according to origin or other features. A quite different pattern of dill seed was found due to the presence of apiol (dill).

Analysis of volatile compounds and metals in essential oil and solvent extracts of Amomi Fructus (사인으로부터 추출한 정유와 용매 추출물의 휘발성 물질 및 금속성분 분석)

  • Lee, Sam-Keun;Eum, Chul Hun;Son, Chang-Gue
    • Analytical Science and Technology
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    • v.28 no.6
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    • pp.436-445
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    • 2015
  • Amomi Fructus with anti-oxidative activity was chosen and essential oil was obtained by SDE (simultaneous distillation extraction), and 39 constituents were determined by GC-MS (gas chromatography-mass spectrometry). Major components were camphor, borneol acetate, borneol, D-limonene and camphene. Three solvent extracts such as hexanes, diethyl ether and methylene chloride from Amomi Fructus were obtained. These were analyzed by GC-MS and 4 more constituents were identified in addition to 39 components discovered in essential oil. Five major components such as camphor, borneol acetate, borneol, D-limonene and camphene were also detected, however the relative peak percents of those components were different from those of constituents in essential oil. To estimate the kind and the amount of materials evaporated at certain temperature and conditions from essential oil and solvent extracts, dynamic headspace apparatus was used and materials evaporated and trapped at certain conditions were analyzed by GC-MS. Recovery yield of SDE method from Amomi Fructus was measured by using camphor and standard calibration solution of camphor methanol solution and, the yield was 82.0%. Content of Hg was measured by mercury analyzer and contents of Cd, Pb, Cr, Mn, Co, Ni, Cu and Zn in Amomi Fructus, essential oils and solvent extracts were determined by ICP-MS (Inductively coupled plasma-mass spectrometer). Pb, Cd and Hg were measured in the concentration of 0.72 mg/kg, <0.10 mg/kg and 0.0023 mg/kg, respectively and these were below permission level of purity test. Contents of Mn, Cu and Zn in Amomi Fructus were 213 mg/kg, 8.29 mg/kg and 31.0 mg/kg, respectively and which were relatively higher than other metals such as Cr, Co and Ni. Metals such as Mn (0.65 ~ 9.08 mg/kg), Cu (1.16 ~ 4.40 mg/kg) and Zn (1.10 ~ 3.80 mg/kg) in essential oil and solvent extracts were detected. At this point it is not clear that the metals were cross-contaminated in the course of treating Amomi Fructus or metals were contained in Amomi Fructus. The influence evaluation toward biological model study of these metals in essential oil and solvent extracts will be needed.

Removal of residual VOCs in a collection chamber using decompression for analysis of large volatile sample

  • Lee, In-Ho;Byun, Chang Kyu;Eum, Chul Hun;Kim, Taewook;Lee, Sam-Keun
    • Analytical Science and Technology
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    • v.34 no.1
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    • pp.23-35
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    • 2021
  • In order to measure the volatile organic compounds (VOCs) of a sample which is too large to use commercially available chamber, a stainless steel vacuum chamber (VC) (with an internal diameter of 205 mm and a height of 50 mm) was manufactured and the temperature of the chamber was controlled using an oven. After concentrating the volatiles of the sample in the chamber by helium gas, it was made possible to remove residual volatile substances present in the chamber under reduced pressure ((2 ± 1) × 10-2 mmHg). The chamber was connected to a purge & trap (P&T) using a 6 port valve to concentrate the VOCs, which were analyzed by gas chromatography-mass spectrometry (GC-MS) after thermal desorption (VC-P&T-GC-MS). Using toluene, the toluene recovery rate of this device was 85 ± 2 %, reproducibility was 5 ± 2 %, and the detection limit was 0.01 ng L-1. The method of removing VOCs remaining in the chamber with helium and the method of removing those with reduced pressure was compared using Korean drinking water regulation (KDWR) VOC Mix A (5 μL of 100 ㎍ mL-1) and butylated hydroxytoluene (BHT, 2 μL of 500 ㎍ mL-1). In case of using helium, which requires a large amount of gas and time, reduced pressure ((2 ± 1) × 10-2 mmHg) only during the GC-MS running time, could remove VOCs and BHT to less than 0.1 % of the original injection concentration. As a result of analyzing volatile substances using VC-P&T-GC-MS of six types of cell phone case, BHT was detected in four types and quantitatively analyzed. Maintaining the chamber at reduced pressure during the GC-MS analysis time eliminated memory effect and did not affect the next sample analysis. The volatile substances in a cell phone case were also analyzed by dynamic headspace (HT3) and GC-MS, and the results of the analysis were compared with those of VC-P&T-GC-MS. Considering the chamber volume and sample weight, the VC-P&T configuration was able to collect volatile substances more efficiently than the HT3. The VC-P&T-GC-MS system is believed to be useful for VOCs measurement of inhomogeneous large sample or devices used inside clean rooms.

Determination of Aroma Components in Pinus densiflora (Pine Needles) Studied by Using Different Extraction Methods (추출방법에 따른 솔잎의 휘발성 성분 조성 비교)

  • Lee Jae-Gon;Lee Chang-Gook;Baek Shin;Kwon Young-Ju;Jang Hee-Jin;Kwag Jae-Jin;Rhee Moon-Soo;Lee Gae-Ho
    • The Korean Journal of Food And Nutrition
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    • v.19 no.2
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    • pp.161-168
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    • 2006
  • The efficiency of six different extraction methods for the analysis of aroma components from pine needle(P. densiflora) was compared by gas chromatography-mass selective detector(GC-MSD). The six methods were dynamic headspace(DHS), reduced pressure headspace(RPHS), solid-phase microextraction(SPME), simultaneous distillation-extraction(SDE), supercritical fluid extraction(SFE) and pyrolysis distillation extraction(PDE). A total of 65 compounds were identified by using the six different extraction methods. These compounds are classified into six categories in terms of chemical functionality: 25 hydrocarbons, 16 alcohols, 9 carbonyls, 6 esters, 7 acids, and 2 ethers. The aroma compounds having low boiling point were more abundant in DHS, RPHS, and SPME extracts. On the other hand, the aroma compounds having high boiling point were more abundants in SDE, SFE and PDE extracts. The acid compounds were extracted by heat-based extraction methods such as SDE, SFE, PDE, but not by DHS, RPHS and SPME, which used neither solvent nor heat. The oxygenated terpens, hexanal, hexanol, and hexadienal were more abundant in DHS and RPHS extracts, compared with the other methods.

Poly(dimethylsiloxane) Mini-disk Extraction

  • Cha, Eun-Ju;Lee, Dong-Sun
    • Bulletin of the Korean Chemical Society
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    • v.32 no.10
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    • pp.3603-3609
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    • 2011
  • A novel sampling method of the headspace poly(dimethylsiloxane) (PDMS) mini-disk extraction (HS-PDE) was developed, optimized, validated and applied for the GC/MS analysis of spices flavors. A prototype PDMS mini-disk (8 mm outer diameter, 0.157 mm thickness, 9.4 mg weight) has been designed and fabricated as a sorption device. The technique uses a small PDMS mini-disk and very small volume of organic solvent and less sample size than the solvent extraction. This new HS-PDE method is very simple to use, inexpensive, rapid, requires less labor. Linearities of calibration curves for ${\alpha}$-pinene, ${\beta}$-pinene, limonene and ${\gamma}$-terpinene by HS-PDE combined with GC/MS were excellent having $r^2$ values greater than 0.99 at the dynamic range of 6.06~3500 ng/mL. The limit of detection (LOD) and the limit of quantitation (LOQ) showed very low values. This method exhibited good precision and accuracy. The overall extraction efficiency of this method was evaluated by using partition coefficients ($K_p$) and concentration factors (CF) for several characteristic components from nutmeg and mace. Partition coefficients were in the range from $2.04{\times}10^4$ to $4.42{\times}10^5$, while CF values were 0.88-15.03. HS-PDE was applied successfully for the analysis of flavors compositions from nutmeg, mace and cumin. The HS-PDE method is a very promising sampling technique for the characterization of volatile flavors.

Flavor Quality of Aroma Fractions Recovered from Peach Pulp (복숭아 펄프에서 회수한 방향성분 획분의 향기특성)

  • Lee, Kyoung-Hae;Lee, Young-Chun
    • Korean Journal of Food Science and Technology
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    • v.27 no.6
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    • pp.921-927
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    • 1995
  • Peach pulp was separated into serum and insoluble pulp by centrifugation at 11,000 rpm for 10 min. The serum portion was concentrated at $50{\sim}55^{\circ}C$ and $30{\sim}50\;mmHg$ with aroma recovery. Vapor generated at the early stage of vacuum evaporation was condensed and taken as aroma fractions: AR-1($0{\sim}5%$), AR-2($5{\sim}10$), AR-3($10{\sim}15%$), AR-4($15{\sim}20%$). Dynamic headspace concentration method was used to trap volatile compounds in aroma fractions and identification of aroma compounds was made by GC/MS. The yield of serum separated from peach pulp was 70.5% and the serum fraction contained the most of aroma compounds. Thirty-one aroma compounds, including ethylene, benzaldehyde, l-limonene and ${\gamma}-dodecalactone$ were identified. The efficiency of aroma recovery was reduced, as the recovery time was extended, as indicated by less peak numbers and peach areas of aroma fractions.

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Aroma Characteristics of Tricholoma matsutake Mushrooms Collected from Eleven Major Sites in Korea (한국(韓國)의 11개(個) 주요(主要) 산지(産地)에서 채집(採集)한 송이(松栮)의 향기성분(香氣成分)에 관(關)한 연구(硏究))

  • Cho, Duck Hyun;Lee, Kyung Joon;Han, Sim Hee
    • Journal of Korean Society of Forest Science
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    • v.88 no.4
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    • pp.490-497
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    • 1999
  • The objectives of this study were to identify aroma characteristics of Tricholoma matsutake(S. Ito et Imai) Sing. growing in different geograghic ranges in South Korea. Mushrooms were collected from 11 major sites which included four sites(Bonghwa, Uljin, Goryung and Chungdo) in Kyongbuk Province, three sites(Changnyung, Hadong and Hamyang) in Kyongnam Province, two sites(Yangyang and Inje) in Kangwon Province, one site(Goisan) in Choongbuk Province, and one site(Namwon) in Chonbuk Province. One of three mushrooms from each site were used for measurements of aromatic characteristics. Aromatic compounds were identified using a dynamic headspace trap method at $40^{\circ}C$ and GC-MSD(gas chromatograph-mass spectrometric detector) method. A total of 25 aromatic compounds were identified. Large variations in the composition and amount of aromatic compounds were noticed. Major aroma compound was 1-octen-3-ol, while methyl cinnamate known as the major aroma compound in matsutake was not detected at all. The total amount of aromatic compounds was highest in Bonghwa, and decreased in the order of Chungdo, Inje, Hamyang, Uljin, and Yangyang. Based on the total amount, kinds and amounts of individual aromatic compounds, the mushrooms from 11 major sites were grouped into following four types : 1) Bongwha Type : the total amount of aromatic compounds was highest, with major compound being 3-methyl 1-butanol. 2) Hamyang Type including Chungdo, Yangyang and Inje : 1-octen-3-of comprised 2/3 of total aromatic compounds, with second major being 3-methyl butanal. 3) Uljin Type : 1-octen-3-ol comprised 94% of total aromatic compounds, with other compounds being almost nothing. 4) Goisan Type including Goryung, Namwon, Changnyung, and Hadong : the total amount of aromatic compounds was lower than other three types.

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