• Title/Summary/Keyword: gas-chromatographic determination

Search Result 99, Processing Time 0.029 seconds

The Selection of Sample Injection Modes and Its Effect on the Calibration Bias in S Gas Detection by Gas Chromatography (GC의 주입방식 차에 따른 고농도 악취황 성분의 검량오차 연구 : 주입부피의 고정방식 대비 주입농도의 고정방식 간 비교연구)

  • Kim Ki-Hyun;Choi YJ
    • Journal of Korean Society for Atmospheric Environment
    • /
    • v.21 no.2
    • /
    • pp.269-274
    • /
    • 2005
  • In this work, analytical bias arising from the gas chromatographic determination of sulfur compounds was evaluated by the application of direct loop injection method to the GC/PFPD detection of four sulfur compounds including H$_{2}$S, CH$_{3}$SH, DMS, and DMDS. For the proper evaluation of analytical uncertainties involved in GC calibration, we employed two comparative techniques of calibration at fxed concentration injection (CFCI) vs calibration at fixed volume injection (CFVI) method. The results of our study indicate that CFCI method exhibits very poor sensitivity due to the matrix effect with varying injection volumes. On the other hand, as CFVI method overcomes such limitation, it can be used to obtain very accurate quantification of S compounds at their high concentration levels above a few to a few tens ppb.

Determination of Sulfur-Containing Odorants in Natural Gas by Gas Chromatography/Flame Photometric Detection (GC/FPD에 의한 천연가스 중 황 함유 부취제의 정량)

  • Choi, Yong-Wook;Kim, Jong-Hun;Choe, Kun-Hyung;Shin, Sung-Sik
    • Analytical Science and Technology
    • /
    • v.7 no.3
    • /
    • pp.349-359
    • /
    • 1994
  • A gas chromatographic method for analyzing the gas odorants concentration in natural gas was studied. Eight odorants involving TBM and THT were completely separated by using OV-10 column. The optimization of several interrelated key parameters affecting the response of FPD such as hydrogen flow rate, air flow rate and detector temperature were accomplished. A permeation device was used to obtain calibration curves of TBM and THT. This analytical method has applied to measure TBM and THT used as a natural gas odorant blend in natural gas pipeline. In order to elucidate the relationship between odor level and odorant level feasibility test of fragrance meter was demonstrated.

  • PDF

Gas Chromatographic Performances for Simultaneous Determination of Multi-pesticide Residues and Extraction of Pesticides with Three Partition Solvents (잔류농약 다성분 동시분석을 위한 기체 크로마토그래피 분석성능과 3종 분배용매에 의한 농약추출)

  • Kim, Chan-Sub;Kim, Jin-Bae;Im, Geon-Jae;Park, Hyun-Ju;Lee, Young-Deuk
    • The Korean Journal of Pesticide Science
    • /
    • v.13 no.3
    • /
    • pp.133-147
    • /
    • 2009
  • In order to develop the simultaneous analytical method for pesticide residues which ones in soil are rapidly and inexpensively measured by, many analytical methods for individual pesticide residue and several methods for multi-pesticide residues in agricultural commodities and food were reviewed. Various gas chromatographic conditions and pre-treatment procedures were intensively investigated and modified. And then new optimum procedure was established and its proficiency was validated. The response on detectors of simultaneous determination of 180 pesticides out of pesticides used in Korea was tested. The number of pesticides that their limits of detection (LOD) equal or lower than $0.05\;mg\;kg^{-1}$ were 137 pesticides on ECD, 170 pesticides on NPD and 179 pesticides on ECD/NPD integrated. The retention times of most pesticides ranged appropriately between 10 minutes and 40 minutes in the proposed chromatographic conditions. But about 90 pesticides eluded between 20 minutes and 30 minutes and so they were not resolved enough. In partition with dichloromethane, ethyl acetate/hexane (1:1) and ethyl acetate, number of pesticides whose extraction efficiency ranged from 70% to 120%, were 163, 154 and 147, respectively.

Determination of Ethylene Oxide Rexidue and its Secondary Products in Powdered Food (분말상 식품에 있어서 Enthylene Oxide의 잔류성과 이차생성물 분석)

  • 권중호;김석원;변명우;조한옥;이기동
    • Journal of Food Hygiene and Safety
    • /
    • v.9 no.1
    • /
    • pp.43-48
    • /
    • 1994
  • Instrumental determination was performed for the analysis of residues of ethylene oxide(EO), ethylene chlorohydrin(ECH) and ethylene glycol(EG) in white ginseng powders which were deaerated for 30 min after EO fumigation. Gas chromatographic data showed that EO residues were 570 ppm in the immediate samples after deaeration and 170 ppm in the stored ones for 8 days at 30$\pm$1$^{\circ}C$, respectively, showing a decreasing tendency with elapsed time. On the other hand, ECH and EG residues in samples as the secondary products of EO were 17, 650 ppm and 727 ppm stored for one month, and 9, 595 ppm and 221 ppm stored for 3 months, respectively.

  • PDF

Organic Pollutant Transport in Unsaturated Porous Media by Atmospheric Breathing Processes( I ) - Partition Coefficient -

  • Ja-Kong;Lim, Jae-Shin;Do, Nam-Young
    • Proceedings of the Korean Society of Soil and Groundwater Environment Conference
    • /
    • 1996.11a
    • /
    • pp.50-53
    • /
    • 1996
  • This paper reports the experimental results for the determination of the overall partition coefficient of VOCs in unsaturated soil, A chromatographic method was used for the determination of gaseous partition coefficients to natural soil under various water content conditions. The equilibrium vapor pressure of water over saturated salt solution was used to fix the relative humidity of the air and control the water content of the soil systems. The transport behavior was studied for dichloromethane, trichloroethane and dichlorobenzene pollutants, with log octanol-water partition coefficients(log $K_{ow}$ ) which range from 1.25 to 3.39, or water to soil partitioning which varies by 135 times; water solubility constants which vary by 3 times; and vapor pressures which range from 1 to 362 torr. Water content of the soil had a pronounced effect on the effective partition coefficient(between gas and soil + water stationary phase) as well as on the effective dispersion coefficient.

  • PDF

Evaluation of soybean oil rancidity by pentanal and hexanal determination (Pentanal과 hexanal 측정에 의한 대두유의 산패도 측정)

  • Chun, Ho-Nam;Kim, Ze-Uook
    • Applied Biological Chemistry
    • /
    • v.34 no.2
    • /
    • pp.149-153
    • /
    • 1991
  • Several commercial soybean oils were stored at $20^{\circ}C,\;40^{\circ}C$ and $60^{\circ}C$ with daily exposure of fluorescent light for 12 hours and evaluated their rancidity by headspace gas chromatographic analysis of pentanal and hexanal. The data of gas chromatographic analysis was compared with organoleptic flavor evaluation. For headspace gas chromatographic analysis, the volatile compounds were recovered by porous polymer trap and flushed into a fused silica capillary column at $250^{\circ}C$, The pentanal and hexanal separated were identified by gas chromatography and gas chromatography-mass spectrometric method. The results showed that the contents of pentanal and hexanal were linearly increased during storage for 100 days. A very simple linear relationship was found between organoleptic flavor scores and amounts of two volatile compounds with very high correlation coefficient. A similar linear relationship was also obtained for acid and peroxide value with sensory data. This results suggested the possible implication of pentanal and hexanal as an quality index for rancidity evaluation of soybean oil.

  • PDF

Determination of trace icing Inhibitors (ether type) in free-floating fuels by gas chromatography-mass spectrometry

  • Shin, Ho-Sang;Ahn, Hye-Sil;Jung, Dong-Gyun
    • Proceedings of the Korean Society of Soil and Groundwater Environment Conference
    • /
    • 2003.04a
    • /
    • pp.196-200
    • /
    • 2003
  • A gas chromatography/mass spectrometric assay method was developed for the simultaneous determination of ethylene glycol monomethyl ether (EGME) and diethylene glycol monomethyl ether (DEGME) in spilled aviation fuels. Ethylene glycol monobutyl ether (EGBE) and ethylene glycol monoethyl ether (EGEE) were used as internal standard and surrogate, respectively. The sample preparation consists of back-extraction with 7 mL of methylene chloride after extraction of 50 mL of fuel with 2 mL of water. The extract was concentrated to dryness and dissolved with 100L of methanol and analyzed by CC-MS (SIM). The peaks had good chromatographic properties by using semi-polar column and the extraction of these compounds from fuel also gave high recoveries of 75 and 85 % with small variations for EGME and DEGME, respectively. Method detection limits were 1.3 ng/mL for EGME and 1.0 ng/mL for DEGME in spilled fuel. The method may be useful for fuel-type differentiation between kerosene and JP-8, which may originate from the storage tank.

  • PDF

Simultaneous Determination of Benzidine, Acetylbenzidine and di-Acetylbenzidine in Rat Urine

  • Sin, Ho Sang;Lee, Jin Hyeon;An, Hye Sil;Hong, Chun Pyo;Choe, Seok Nam
    • Bulletin of the Korean Chemical Society
    • /
    • v.22 no.7
    • /
    • pp.685-688
    • /
    • 2001
  • A gas chromatography/mass spectrometric assay method has been developed for the simultaneous determination of benzidine (BZ), N-acetyl benzidine (ABZ) and N,N-diacetyl benzidine (DABZ) in rat urine. BZ, ABZ and DABZ were extracted from urine at pH 8 with ethyl ether. Conjugated urinary metabolites were extracted at pH 8 after hydrolysis with 1 M HCl for 30 min at 100 $^{\circ}C.$ The dried extract was dissolved in 100 ${\mu}{\ell}$ of ethylacetate and then injected in gas chromatography-mass spectrometric (GC-MS) system without further purification or modification. BZ, ABZ and DABZ have good chromatographic properties and offer very sensitive response for the EI-MS (SIM) without any derivatization. The recoveries for BZ, ABZ and DABZ were about 98.0, 81.8 and 71.4%, respectively, at pH 8.0 and the concentration of 5.0 ng/mL. The coefficients of variation of BZ and ABZ were less than 9.5% from 0.1 to 100 ng/mL and that of DABZ was less than 13% in the same concentration range. The detection limits of the assay were 0.01 ng/mL for both BZ and ABZ, and 0.05 ng/mL for DABZ in urine or plasma 1.0 mL.

A Study on the Simplified Extraction and Cleanup Technique for Organophosphorus and Organochlorine pesticides in Vegetables (채소 중의 유기인제 및 유기염소제 농약의 단순화된 抽出과 精製 技法에 관한 연구)

  • 전옥경;이용욱
    • Journal of Environmental Health Sciences
    • /
    • v.23 no.1
    • /
    • pp.66-73
    • /
    • 1997
  • This procedure describes the method for gas chromatographic determination of 31 organophosphorus and 28 organochlorine pesticides in 10g of spinach, tomato and onion. After the pesticides were extracted with several solvents, the amount of coextractives and recovery rates of acephate and methamidophos were calculated. Samples for organochlorine pesticides were cleaned up with florisil solid phase extraction columns. NaBH$_4$ was added to onion extracts, which contained sulfur compound. All the concentrated extracts were analyzed by gas chromatography with ECD and NPD. The smallest amount of coextractives resulted from the spinach samples extracted with 5% MeOH in ethyl acetate. 5% EOH in ethyl acetate had the highest extractability for acephate and methamidophos and gave the best overall performance as an extraction solvent. The ability of 5% EOH in ethyl acetate to extract various organophosphorus and organochlorine pesticides from spinach, tomato and onion was examined. Recovery of 59 insecticides ranged from 58.0% to 110.5%. The average recoveries of fortified spinach, tomato and onion were 90.08%, 94.54% and 84.90%, respectively.

  • PDF

Volatile Free Acid Profiling of Body Fluids by Gas Chromatography (기체 Chromatograph를 이용한 체액내 Volatile Free Acid의 분석연구)

  • Kim, Kyoung-Rae;Hahn, Mi-Kyoung
    • YAKHAK HOEJI
    • /
    • v.32 no.1
    • /
    • pp.6-13
    • /
    • 1988
  • A gas chromatographic method is described for the determination of volatile free acids(VFAs) in body fluids. VFAs were trace enriched from body fluids by liquid-solid extraction using Chromosorb P as the solid sorbent and ether as the eluant. The enriched VFAs were injected in splitless injection mode onto a HP-20M fused silica capillary column. The flame ionization detector was used as the detector. The present method was applied to the profiling of VFAs in body fluids from patients suffering from the infectious disease, hepatitis. The VFAs concentrations were high in saliva of hepatitis patients and isobutyric acid detected in sera of hepatitis patients compared to healthy subjects.

  • PDF