• Title/Summary/Keyword: GC/O

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Analysis of Imidazoline Type Cationic Surfactants (Imidazoline계 양이온 계면활성제 분석)

  • Bak, Hong-Soon;Choi, Kyu-Yeol;Lee, Jae-Duk;Kim, Yeo-Kyung;Ahn, Ho-Jeong
    • Applied Chemistry for Engineering
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    • v.9 no.3
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    • pp.404-406
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    • 1998
  • Analysis for the imidazoline type cationic surfactants was performed by the gas chromatography(GC) and high performance liquid chromatography(HPLC). The composition of the alkyl chain distribution was investigated by GC after base/Acid hydrolysis of the imidazoline ring. The distribution of total alkyl chain was separated clearly by a Bondclone C18/NOVA-Pak C18 HPLC column using 50% acetonitrile in methanol containing 0.1M sodium perchlorate as a mobile phase. Alkyl chain distribution and average molecular weight of imidazoline type cationic surfactants were obtained based on these analytical methods. The agreement of results from GC and HPLC was good. The detection limit of imidazoline by HPLC method was 10ng without pretreatment.

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Development and validation of a qualitative GC-MS method for THCCOOH in urine using injection-port derivatization

  • Sim, Yeong Eun;Kim, Ji Woo;Kim, Jin Young
    • Analytical Science and Technology
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    • v.34 no.2
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    • pp.68-77
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    • 2021
  • Cannabis is one of the most abused drugs in Korea. The main psychoactive component in cannabis, Δ9-tetrahydrocannabinol, is metabolized to 11-nor-9-carboxy-Δ9-tetrahydrocannabinol (THCCOOH) and THCCOOH-glucuronide (THCCOOH-glu) in the human liver, whereby the amount of THCCOOH-glu found in urine is twice as high as that of THCCOOH. The analytical process adapted by the majority of urine drug-testing programs involves a two-step method consisting of an initial immunoassay-based screening test followed by a confirmatory test if the screening test result is positive. In this study, a qualitative gas chromatography-mass spectrometry (GC-MS) method was developed and validated for the detection of THCCOOH in human urine, where THCCOOH-glu was converted into THCCOOH by alkaline hydrolysis. For purification of the urine extract prior to instrumental analysis, high-speed centrifugation was used to minimize interference. In addition, an injection-port derivatization method using ethyl acetate and N,O-bis(trimethylsilyl)-trifluoroacetamide containing 1 % trimethylchlorosilane was employed to reduce the time required for derivatization, and an aliquot of the final solution was injected into the GC-MS. The method was validated by measuring the selectivity, limit of detection (LOD), and repeatability. The sensitivity, specificity, precision, accuracy, Kappa, F-measure, false positive, and false negative rate were determined by comparing the GC-MS results with those obtained using the immunoassay. The LOD was determined to be 0.32 ng/mL, while the repeatability was within 9.1 % for THCCOOH. Furthermore, a comparison study was carried out, whereby the screening immunoassay exhibited a sensitivity of 86.4 % and a specificity of 100 % compared to GC-MS. The applicability of the developed method was examined by analyzing spiked urine and forensic urine samples obtained from suspected cannabis abusers (n = 221).

Determination of 25 EDs in Frog and Fish Tissue by GC-MS (SIM)

  • Shin, Ueon-Sang;Shin, Ho-Sang
    • Bulletin of the Korean Chemical Society
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    • v.24 no.4
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    • pp.413-420
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    • 2003
  • A gas chromatography/mass spectrometric assay method was developed for the simultaneous determination of neutral and bacis twenty-five disruptors $(ED_S)$ in frog and fish. Afther homogenization and sonication of 5 g of sample, purification was achieves in one step with a solid phase extraction procedure using silica gelflorisl. Eluton was performed with 50mL of acetone : n-hexane (1 : 9) solution. The eluate was concentrated to approximately 10uL and dissolves with 100 uL of hexane and analyzed by GC-MS (SIM). The peaks had good chromatographic properties and the extraction of these compounds from sample also gave relatively high recoveries with small variatoins. Detection limits were 0.1 ng/g for 4-nitrotoluene, benzophenone, hexachlorobenzene, atrazine, malathion, o,p-DDT, o,p-DDT and permethrin, and 0.2 ng/g for heptachlor epoxide, γ-chlordane, α-chlordane, p,p'-DDE, p,p'-DDD, cypermethrin and fenvalerate, and 0.3 ng/g for trifluralin, metribuzin, alachlor, dieldrin and p,p'-DDT, and 0.5 ng/g for heptachlor, aldrin and parathion, and 0.7 ng/g for endrin, and 0.8 ng/g for nitrofen. The recoveries were between 33 and 109%. The method was used to analyze twenty-five frogs and forty-six fishes fishes samples caught from various regions in Korea. Benzophenone was detected at concentration of up to 17.2 ng/g in frog or fish. Heptachlor, aldrin, γ-chlordane, p,p'-DDE, p,p'-DDD, endrin and o,p-DDD were detected at concentrations of 0.7-12.5 ng/g in frog or fish. Also significant leveles of dieldrin (up to 22.5 ng/g) were observed. The developed method may be valuable to be used to the national monitoring project of EDS in biota samples.

A Study on the Identification of Hazardous Organic Substances for Industrial Classification (업종별 유해성 유기물질의 확인에 대한 연구)

  • Park, Sun Ku;Kim, Sung Soo;Ko, O Suk;Jung, Sung Woong;Park, Jun Dae;Ryu, Seung Do;Ryu, Jae Kyun;Cho, Hyun-Woo
    • Analytical Science and Technology
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    • v.9 no.4
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    • pp.392-398
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    • 1996
  • Eleven organic chemical substances, tetrachloroethylene, ethyl benzene, p-xylene, o-xylene, isopropyl benzene, n-propyl benzene. 1,2,4-trimethyl benzene, 1,3,5-trimethyl benzene, p-isopropyl toluene. see-butyl benzene, and naphthalene, which have hazardously influenced to human, were extracted from untreated wastewater collected at 26 companies of 8 types industry in the basin of Kwangju stream. Their structures were elucidated by Gas Chromatography/Mass Spectrometry(GC/MS) and in comparison with each standard reagents.

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Determination of Cr(Ⅵ) by Glassy Carbon and Platinum Electrodes Modified With Polypyrrole Film (폴리피롤 막으로 변성시킨 유리질 탄소 및 백금 전극에서 Cr(Ⅵ) 이온의 정량)

  • Yoo, Kwang Sik;Woo, Sang Beom;Jyoung, Jy Young
    • Journal of the Korean Chemical Society
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    • v.43 no.4
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    • pp.407-411
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    • 1999
  • Studies have been carried out on the fabrication of PPy/GC and PPy/Pt electrode modified with polypyrrole film and determination of Cr(VI) by using 3-electrode system with modified electrodes. Modified electrodes were able to easily fabricated by cyclic voltammetry scanned from +1.0V to -1.0V(vs. Ag/AgCl) at 50 mV/sec. Film thickness could be controlled at same condition by the number of cycling up to 26 times. Reduction behaviour of Cr(VI) at PPy/GC electrode could be seen at wide potential ranges from +0.6V to -0.5V(vs. Ag/AgCl), and maximum reduction peak potential of the ion was observed at -0.25V(vs.Ag/AgCl). Calibration graph at its potential was linear from 0.1 ppm to 80.O ppm. Slope factor and relative coefficient were 1.75 mA/ppm and 0.998, respectively. Reduction behaviour of Cr(VI) at PPy/Pt electrode was similar to PPy/GC electrode, Calibration graph was linear from l.0 ppm to 60.0 ppm. Slope factor and relative coefficient were 0.5mA/ppm and 0.923, respectively. But PPy/GC modified electrode had about 3 times higher sensitivity than PPy/Pt modified electrode. Reduction behaviour of Cu(II), As(IlI), Pb(II), and Cd(II) couldn't be seen at PPy/GC electrode,Its metals had not lnterfered with Cr (VI) determination.

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Selective Production of Monomeric Phenols from Lignin via Two-step Catalytic Cracking Process (2단계 촉매 분해공정을 이용한 리그닌 유래 선택적 페놀화합물 생산)

  • Kim, Jae-Young;Heo, Sujung;Park, Shin Young;Choi, In-Gyu;Choi, Joon Weon
    • Journal of the Korean Wood Science and Technology
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    • v.45 no.3
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    • pp.278-287
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    • 2017
  • In this study, lignin was efficiently degraded via two-step catalytic cracking process and lignin-oil, char, and gas was produced as lignin degraded products. Three kinds of catalysts (MgO, CaO, and Pt/C) were used in first catalytic cracking step and the highest lignin-oil yield (76.2 wt%) was obtained in Pt/C catalyst with the smallest char formation (4.1 wt%). GC-MS/FID analysis revealed that 18 kinds of monomeric phenols existed in lignin-oil and sum of them was the highest in Pt/C condition (97.8 mg/g lignin). Meanwhile, relatively lower yield of monomeric phenols was produced in MgO and CaO condition because of their absorption on catalysts. Lignin-oil produced over Pt/C was introduced to second catalytic cracking process with porous Pd/activated carbon aerogel catalyst. From this process, four kinds of monomeric phenols such as 4-ethylguaiacol, 4-propylguaiacol, 4-ethylsyringol, 4-propylsyringol were selectively produced at 0.89 - 1.82 wt% level.

The review on standard method of microplastics in soil and groundwater (토양, 지하수 중 미세플라스틱 분석법에 관한 고찰)

  • JongBeom Kwon;Hyeonhee Choi;Sunhwa Park
    • Analytical Science and Technology
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    • v.37 no.3
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    • pp.174-188
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    • 2024
  • This review summarized research trends regarding sample collection methods, pretreatment method, and types of analysis devices for microplastics (MPs) in soil and groundwater matrices. Soil sampling considers the selection of sampling location, depth, and volume. The typically sampling depth is within 15 cm (topsoil), and about 1 kg of mixed each sample. Among spot sampling and continuous flow sampling, groundwater sampling mainly used a continuous flow sampling, with collection rates 2 to 6 L/min in the range of 300~1,000 L, and followed by immediate on-situ filtration. Pretreatment method, applied to soil and groundwater, consist of organic digestion and density separation. In the organic digestion method, H2O2 is recommended among H2O2, acidic, alkaline, and enzymatic method. NaCl is primarily used as a reagent in density separation. However, depending on the density of MPs, other regents can be selectively used like ZnCl2, ZnBr2, and etc. Representative analysis device includes Fourier Transform Infrared (FTIR) and Raman spectroscopy for non-destructive analysis and Pyrolysis Gas Chromatography Mass Spectrometry (Py-GC/MS) for destructive analysis. µ-FTIR and Raman can count MPs of larger than 10 and 1 ㎛, and analyze MPs materials. However, it is need to sufficiently remove interference, like organic matter, in spectroscopic analysis using essential pretreatment method. Py-GC/MS is being continuously researched because it doesn't require complex pretreatment method and allows quantitative analysis of specific materials.

Comparison of Volatile Components in Fresh and Dried Red Peppers (Capsicum annuum L.)

  • Jun, Hae-Roung;Cho, In-Hee;Choi, Hyung-Kyoon;Kim, Young-Suk
    • Food Science and Biotechnology
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    • v.14 no.3
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    • pp.392-398
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    • 2005
  • Fresh, and sun- and oven-dried red peppers were analyzed for volatile components. Also, their odor-active compounds were determined using gas chromatography-olfactometry (GC-O). More diverse volatile components, such as aldehydes, ketones, acids, and esters, were found in dried samples than in fresh ones. They included hexanal, ethyl acetate, ${\alpha}$-ionone, and ${\beta}$-ionone. Some Strecker aldehydes, 2-methyl butanal and 3-methyl butanal, were found only in dried red peppers. More hydrocarbons of high volatility and terpene-type components, such as ${\gamma}$-terpinene and aromadendrene, were detected only in fresh red peppers. A considerable amount of naphthalene was formed during sun-drying, whereas 2-furancarboxaldehyde, 1-methyl-1H-pyrrole and benzeneethanol were detected only in oven-dried red peppers. Characteristic odor of fresh ones could be attributed to 3-penten-2-o1, 2-methyl-2-butenal, 2-methoxy phenol, 2-hydroxy-methyl-benzoate, and 2-phenoxy ethanol, whereas some odorants, including 2-pentyl furan, naphthalene, hexyl hexanoate, and ${\alpha}$-ionone, could be responsible for distinctive odor property of sun-dried red peppers. 2-Furancarboxaldehyde, benzeneethanol, 4-vinyl-2-methoxy phenol, and unknown played important roles in odor property of oven-dried red peppers.

The Adsorption Removal Characteristics of Trace Organic By-Products in Disinfection of Drinking Water by Biological Activated Carbon(BAC) (음용수 소독 미량 유기오염물질 생성에 대한 생물활성탄(Biological Activated Carbon)의 흡착제거 특성)

  • Ok, Chi-Sang;Kim, Jeong-A;Bae, Gi-Cheol
    • Journal of Environmental Science International
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    • v.1 no.1
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    • pp.53-68
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    • 1992
  • In order to research the adsorption removal characteristics of trace organic by-products in disinfection of drinking water by biological activated carbon(BAC), water samples disinfect- ted with $Cl_2$, $O_3$ and $ClO_2$ after treatment by fluidized-bed system with water added with humic acid(10mg/L) were investigated the formation and the removal of trihalomethanes (THMs), and the trace organic by-products by gas chromatography(GC) II gas chromatography/mass selective detector(GC/MSD). Control was used by activated carbon(AC) and water added with humic acid(HA). The results were summarized as follow : The THMs removal effect of BAC by chlorination was in lower 90 % than that of control(HA), the sorts of oxidants formed by $Cl_2$ , $O_3$ and $ClO_2$ were that $O_3$ was very fewer than $Cl_2$ or $ClO_2$, and that $ClO_2$ was fewer than $Cl_2$. The trace organic by-products were esters and phthalates etc. Based on results above, it is concluded that BAC was appeared the more desirable adsorbtion-degradation removal characteristics than that of AC.

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Decomposition Study of Acetaldehyde by Metal-oxide Catalysts (금속산화물 촉매에 의한 $CH_3CHO$의 분해반응 연구)

  • Lee, Chang-Seop;Kim, Young-Eun;Choi, Sung-Woo
    • Journal of the Korean Institute of Gas
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    • v.11 no.2 s.35
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    • pp.25-30
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    • 2007
  • The catalysts for decomposition reaction of acetaldehyde were investigated. The catalysts were prepared with transition metal Ni, Mo, Al on ${\gamma}-Al_2O_3$ support by impregnation method. Physio-chemical properties of catalysts were characterized by SEM-EDS, XRD, XPS, BET and TPR techniques. The conversion efficiency of catalysts for acetaldehyde was measured in the temperature range of $150{\sim}500^{\circ}C$ by GC through the micro reactor system. The 8 wt% $Ni/{\gamma}-Al_2O_3$ was found to be the most active catalyst of mono-metal catalysts tested, and the 1-3 wt% $Ni-Al/{\gamma}-Al_2O_3$ showed higher conversion efficiency than other bimetallic catalysts.

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