• Title/Summary/Keyword: headspace sample

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$KMnO_4$를 이용한 TCE 제거 실험 연구(I): -Headspace sample과 liquid sample 분석과 비교-

  • 현승규;우남칠;최인혁;이기철
    • Proceedings of the Korean Society of Soil and Groundwater Environment Conference
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    • 2004.04a
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    • pp.370-375
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    • 2004
  • KMnO$_4$에 의한 TCE 용액의 분해에서 Headspace를 가진 반응 용기는 liquid sample을 headspce의 관측값으로 반응의 특성을 나타낼 수 없다. 이런 특성에 의해 in-situ KMnO$_4$ 이용은 TCE의 제거 효율에서 자연적인 휘발을 고려해야한다. 1:2.45 몰비에서 liquid sample의 결과 반감기는 약 80분이고 160분에 약 67%의 제거율을 보인다. 1:12.27 몰비의 경우 반감기는 10분이고 90분에 95%의 제거효율을 보인다.

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Headspace Hanging Drop Liquid Phase Microextraction and Gas Chromatography-Mass Spectrometry for the Analysis of Flavors from Clove Buds

  • Jung, Mi-Jin;Shin, Yeon-Jae;Oh, Se-Yeon;Kim, Nam-Sun;Kim, Kun;Lee, Dong-Sun
    • Bulletin of the Korean Chemical Society
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    • v.27 no.2
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    • pp.231-236
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    • 2006
  • A novel sample pretreatment technique, headspace hanging drop liquid phase microextraction (HS-LPME) was studied and applied to the determination of flavors from solid clove buds by gas chromatography-mass spectrometry (GC-MS). Several parameters affecting on HS-LPME such as organic solvent drop volume, extraction time, extraction temperature and phase ratio were investigated. 1-Octanol was selected as the extracting solvent, drop size was fixed to 0.6 $\mu$L. 60 min extraction time at 25 ${^{\circ}C}$ was chosen. HS-LPME has the good efficiency demonstrated by the higher partition equilibrium constant ($K_{lh}$) values and concentration factor (CF) values. The limits of detection (LOD) were 1.5-3.2 ng. The amounts of eugenol, $\beta$-caryophyllene and eugenol acetate from the clove bud sample were 1.90 mg/g, 1.47 mg/g and 7.0 mg/g, respectively. This hanging drop based method is a simple, fast and easy sample enrichment technique using minimal solvent. HSLPME is an alternative sample preparation method for the analysis of volatile aroma compounds by GC-MS.

Headspace Hanging Drop Liquid Phase Microextraction and GC-MS for the Determination of Linalool from Evening Primrose Flowers

  • Kim, Nam-Sun;Jung, Mi-Jin;Yoo, Zoo-Won;Lee, Sun-Neo;Lee, Dong-Sun
    • Bulletin of the Korean Chemical Society
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    • v.26 no.12
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    • pp.1996-2000
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    • 2005
  • Headspace hanging drop liquid phase micro-extraction (HS-HD-LPME) is studied as a novel solvent-based sample pretreatment method for floral volatile aroma compounds. This paper reports on application of the HSHD- LPME combined with GC-MS for the analysis of linalool component emitted from evening primrose flowers. The effect of several variables on the method performance was investigated. Additionally, the separation of enantiomers on a cyclodextrin capillary column was performed to identify chirality of (−)-linalool component. Since the unsurpassed volume of a few micro-liters of solvent is used, there is minimal waste or exposure to toxic organic solvents. This method enables to combine extraction, enrichment, clean-up, and sample introduction into a single step prior to the chromatographic process.

A Modified Method for the Determination of the Carboxyl Groups in Fibers by Headspace Gas Chromatography

  • Hou, Qingxi;Chai, Xin-Sheng;Zhu, Junyong
    • Proceedings of the Korea Technical Association of the Pulp and Paper Industry Conference
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    • 2006.06b
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    • pp.265-270
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    • 2006
  • This paper reports an improved headspace gas chromatographic method for the determination of carboxyl group content in wood fibers. Pretreatment of wood fibers was applied using dilute HCl to convert carboxyl groups to carboxylic acid groups and then using deionized water to wash fiber samples thoroughly. The samples were finally air dried. Sodium bicarbonate solution was used to react with carboxylic acid groups of the pretreated fibers in a closed testing vial to release carbon dioxide. The content of carboxyl groups in fibers was accurately quantified by determining the amount of carbon dioxide released by a headspace gas chromatograph equipped with a thermal conductivity detector. The modified process for fiber sample pretreatment increased the reliability and accuracy in measuring carboxylic acid groups. The present method is simple, accurate.

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Optimization of Dynamic Headspace Purge Conditions for Concentration of Volatile Flavor Compounds of Roasted Perilla Seeds Oil by Response Surface Methodology (반응표면 분석에 의한 볶음들기름의 향기성분 포집조건 최적화)

  • Kim, Suk-Ju
    • The Korean Journal of Food And Nutrition
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    • v.17 no.2
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    • pp.220-228
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    • 2004
  • Dynamic headspace purge conditions were investigated to obtain minimum loss of high volatile compounds by breakthrough and maximum recovery of low volatile components of roasted perilla seed oil (RPSO). A response surface methodology was applied to evaluate the effect of purge temperature, purge time, and sample weight on $\ell$ n (total peak area), breakthrough ratio, and peak area of perilla ketone the least volatile component of RPSO. Sample weight was the most important factor on the $\ell$ n (total peak area) but it did not affect peak area of perilla ketone. All process variables significantly influenced breakthrough ratio. The optimum condition was determined by superimposing contour plots at purge temperature of 48$^{\circ}C$ for 12 min purge time at sample weight of 0.60 g. 2-Propanone, 2-butanone, acetic acid, 2-methyl propanal were main breakthrough compounds in RPSO flavor.

Determination of MTBE, TBA and BTEX in Soil by Headspace Gas Chromatography-Mass Spectrometry

  • Shin, Ho-Sang
    • Bulletin of the Korean Chemical Society
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    • v.33 no.5
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    • pp.1693-1698
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    • 2012
  • A headspace gas chromatographic mass spectrometric (GC-MS) assay method was developed for the simultaneous determination of methyl tertiary butyl ether (MTBE), $tert$-butyl alcohol (TBA) and benzene, toluene, ethyl benzene and xylene (BTEX) in soil contaminated with gasoline. 2 g of soil sample were placed in a 10 mL headspace vial filled with 5 mL of phosphoric acid solution (pH 3) saturated with NaCl, and the solution was spiked with fluorobenzene as an internal standard and sealed with a cap. The vial was heated in a heating block for 40 min at $80^{\circ}C$. The detection limits of the assay were 0.08-0.12 ${\mu}g$/kg for the analytes. For five independent determinations at 10 and 50 ${\mu}g$/kg, the relative standard deviations were less than 10%. The method was used to analyze fifty six soil samples collected from various regions contaminated with gasoline in Korea. The developed method may be valuable for the monitoring of the analytes in soil.

Optimization of Headspace Analysis of Volatile Compounds from Oxidized Fish Oil

  • Shin, Eui-Cheol;Jang, Hae-Jin;Lee, Hyung-Il;An, Hae-Jung;Lee, Yang-Bong
    • Preventive Nutrition and Food Science
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    • v.8 no.4
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    • pp.315-320
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    • 2003
  • Headspace volatile compounds of oxidized fish oil were analyzed by the combination of hexane solvent or solid phase microextraction, gas chromatography and mass selective detector. The optimum condition of headspace analysis by hexane trapping was 23 min absorption time, 96$^{\circ}C$ sample temperature and 20 mL/min air flow rate. The numbers of volatile compounds identified by solvent trapping and SPME were 35 and 14, respectively. Groups having the largest amount and many kinds were hydrocarbons and aldehydes, respectively. The numbers of aldehydes were 15 and 6 for solvent trap and SPME, respectively. These basic data could be used as indicators for the quality changes of fish oil.

Measurement of 1,4-dioxane in surface water by headspace GC-MS (GC-MS에 의한 지표수에서 1,4-Dioxane의 측정)

  • Hong, Seon-Haw;Lee, Jun-Bae;Lee, Soo-Hyung;Lim, Hyun-Hee;Shin, Ho-Sang
    • Analytical Science and Technology
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    • v.27 no.1
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    • pp.22-26
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    • 2014
  • 1,4-Dioxane was classified as a Group 2B carcinogen by the International Agency for Research on Cancer. The compound was measured in surface water with a headspace gas chromatographic mass spectrometric detection. A 5 mL water sample was placed in a 10 mL headspace vial and saturated with NaCl, and the solution was spiked with 1,4-dioxane-d8 as an internal standard and sealed with a cap. Water samples were collected from twenty-two basins of Gum-River on June and September 2012, respectively. As a result, 1,4-dioxane was detected in the concentration range of $0.49-43.0{\mu}g/L$ (mean $2.0{\mu}g/L$) in the frequency of about 30% in surface water samples.

Analysis of Benzene in Beverages by Headspace-GC/MS (Headspace-GC/MS를 이용한 음료 중 벤젠 분석)

  • Kim, Eun-Ju;Park, Sang-Aeh;Choi, Dong-Mi
    • Journal of Food Hygiene and Safety
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    • v.22 no.4
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    • pp.243-247
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    • 2007
  • A selective analytical method of headspace-GC/MS has been applied to determine levels of benzene in beverages. Food samples were 85 including 2 fruit juices, 6 fruit beverages, 11 carbonated beverages, 55 mixed beverages, and 4 beverage concentrations, and 7 extracted beverages. For phase equilibration of headspace, sample was stirred at $40^{\circ}C$ for 30 min. The oven temperature was $60^{\circ}C$ and elevated to $180^{\circ}C$ at $15^{\circ}C/min$. The internal standard was benzene-d6. The identification was done by the selected target ions such as m/z 51, 77, and 78 and the confirmation was done by the response ratio of m/z 77 to m/z 78 between sample and standard. The overall recoveries were ranged from 91% to 101% and the limit of quantification was $1{\mu}g/kg$. The average level of benzene were $5{\mu}g/kg$ for fruit beverages, $2{\mu}g/kg$ for carbonated beverages, $7{\mu}g/kg$ for mixed beverages and $7{\mu}g/kg$ for extracted beverages.