• Title, Summary, Keyword: GC/MS

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Analysis of ambers with different origin by IR and py/GC/MS (산지별 호박(amber)의 IR 및 py/GC/MS 특성 분석)

  • Park, Jong-Seo;Lim, Yu-Jin
    • Analytical Science and Technology
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    • v.24 no.4
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    • pp.256-265
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    • 2011
  • Ambers have been used as a gemstone and a religious object since the ancient times and found in several archaeological sites in Korea. To prepare an enhanced conservation measures, we surveyed the chemical and spectroscopic properties of the ambers according to the provenance. Total 14 amber samples were collected from 6 different provenances including Baltic, Chiapas, Colombian, Dominican, Fushun and Madagascar amber. Infrared (IR) spectroscopic analysis was conducted for the non-destructive examination of the amber samples. They were also analyzed with pyrolysis/GC/MS (py/GC/MS) at the pyrolysis temperature of $300^{\circ}C$ with the on-line derivatization to trimethylsilyl ester. Baltic shoulder corresponding to the absorption at $1250cm^{-1}{\sim}1150cm^{-1}$ appeared in the IR spectrum of Baltic amber. IR spectra of the other ambers also showed somewhat distinctive characteristic peaks. In py/GC/MS analysis peaks assignable to succinic acid, dehydroabietic acid and pimaric acid were detected, which are known to be the components of the amber. In the meanwhile, the presence of compounds appearing in certain amber will be applied to differentiate the provenances of amber relics if their fragments are available for the analysis. These results are expected to help the confirmation of archaeological amber relics and archaeometric interpretation of provenances and manufacturing techniques.

Determination of Nicotine and Other Minor Alkaloids in Tobacco Leaves by GC/MS (GC/MS를 이용한 잎담배 중 알칼로이드 함량 분석)

  • Lee Jeong-Min;Min Hye-Jung;Kim Yong-Ha;Rhee Moon-Soo
    • Journal of the Korean Society of Tobacco Science
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    • v.27 no.1
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    • pp.100-106
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    • 2005
  • To obtain the optimum condition for analysis of 10 alkaloids in tobacco leaves, such as nicotine, nornicotine, anatabine, anabasine, myosmine, cotinine, 2,3'-dipyridyl, $\beta-nicotyrine,\;\beta-nornicotyrine\;and\;\beta-formylnornicotin$, 5 types of extraction method were investigated by GC-FID and GC/MS. The optimum condition of alkaloid extraction was achieved by using methanol:dichloromethane(1:3, v/v) after NaOH treatment. The use of mass selective detector (MSD) provided unambiguous nicotine related alkaloid analysis. Alkaloids in various tobacco leaves were extracted with the optimum extraction condition and quantified by GC/MS/SIM mode. Compared with concentrations of alkaloids among the various tobacco leaves, the concentration of alkaloids was generally in the order burley > flue-cured > oriental tobacco. In flue-cured tobacco leaves, the order of concentration of alkaloids was nicotine > anatabine > nornicotine > $\beta-nicotyrine\;>\;\beta-formylnornicotine\; >\;myosmine\;>\;2,3'-dipyridyl\;>\;cotinine\;>\;anabasine\;>\;\beta-nornicotyrine$. However, in the case of burley and oriental tobacco leaves, the concentration of nornicotine was higher than that of anatabine.

Multivariate Analysis and Gas Chromatographic Determination of the Smelly Nitro Compounds in Dried-Fishes (GC에 의한 건어물 냄새성분중 질소화합물 분석과 다변량해석)

  • Bae, Sun Young;Lee, Dong Sun
    • Journal of the Korean Chemical Society
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    • v.41 no.2
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    • pp.105-112
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    • 1997
  • The smelly nitro compounds were extracted from dried fishes by simultanous distillation and extraction, then were analyzed by GC-MS. Carbon number and order of an amine could be predicted by using retention time and equivalent chain length. Anchovy, codfish, imitation crab meat, cuttle fish, file fish, pollack, shrimp, octopus, harvest fish, and hard-shelled mussel were used for this investigation. Various smelly nitro compounds such as methylamine, acetamide, thiazole, 2-hydroxy isopropylamine, N-methyl pyrroline, piperidine, cyclohexylamine were identified, however, dimethylamine, trimethylamine, diethylamine were not detected. Principal components analysis was applied to GC-MS profiles for pattern recognition of smelly nitro compounds in dried fishes. Multivariate aspects using principal components analysis were very useful for pattern recognition of smelly components, category similarity.

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Determination of Quintozene Residues in Agricultural Commodities Using GC-ECD/MS (GC-ECD/MS를 이용한 농산물 중 Quintozene의 잔류분석)

  • Ahn, Kyung-Geun;Kim, Gyeong-Ha;Kim, Gi-Ppeum;Hwang, Young-Sun;Hong, Seung-Beom;Lee, Young Deuk;Choung, Myoung-Gun
    • The Korean Journal of Pesticide Science
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    • v.19 no.3
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    • pp.195-203
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    • 2015
  • Quintozene, pentachloronitrobenzene (PCNB) is a contact fungicide for control of soilborne phytopathogenic fungi during cultivation of diverse crops. It was introduced to agricultural use around 1930's as a substitute for mercurial disinfectants. Although quintozene had been first registered in Korea on 1969. However, now it was banned to use due to its high residue levels in selected harvest products. Also, high possibility is expected that the residue may be contained in imported agricultural commodities as it is still used widely over the world. Therefore, this study was conducted to establish a determination method for quintozene residue in crops using GC/ECD/MS. Quintozene residue was extracted with acetonitrile from representative samples of five raw products which comprised hulled rice, soybean, Kimchi cabbage, green pepper, and apple. The extract was diluted with saline water, and n-hexane partition was followed to recover quintozene from the aqueous phase. Florisil column chromatography was additionally employed for final clean up of the extract. The quintozene was quantitated by GLC with ECD, using a DB-1 capillary column. The crops were fortified with quintozene at 3 levels per crop. Mean recoveries ranged from 79.9% to 102.7% in five representative agricultural commodities. The coefficients of variation were less than 4.3%. Quantitative limit of quintozene was 0.004 mg/kg in representative five crop samples. A GC/MS with selected-ion monitoring was also provided to confirm the suspected residue. Therefore, this analytical method was reproducible and sensitive enough to determine the residue of quintozene in agricultural commodities.

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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Synthesis of DMDBTDMA and determination of radiolysis products by GC/MS (DMDBTDMA의 합성 및 방사선 분해산물의 GC/MS 분석)

  • Yang, Han-Beom;Lee, Eil-Hee;Park, Gyo-Beom
    • Analytical Science and Technology
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    • v.21 no.5
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    • pp.403-411
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    • 2008
  • Dimethyldibutyltetradecylmalonamide (DMDBTDMA) extractant was used in a solvent extraction process for a radioactive liquid waste treatment. For the study of radiolysis phenomena, DMDBTDMA was synthesized and the degradation compounds (n-methylbutylamine, tetradecane, 1-tetradecanol) in the DMDBTDMA extractant, irradiated with $^{60}Co$ gamma ray, were identified and determined as radiolysis products by a Fourier transform infrared (FT-IR), gas chromatograph/mass spectrometer (GC/MS) analysis and GC/MS with selected ion monitoring (SIM) mode. Retention behavior of n-methylbutylamine, n-dodecane, tetradecane and 1-tetradecanol in the total ion chromatogram with the standard materials and n-dodecane as the internal standard (ISTD) were 2.35 min., 8.83 min., 10.68 min. and 12.75 min., respectively. In the case of tetradecane, there was a linear relationship between the concentration of the tetradecane and the absorbed dose of the ${\gamma}$-ray irradiated DMDBTDMA.

Analysis of animal glue by pyrolysis/GC/MS (열분해/GC/MS에 의한 아교의 분석)

  • Park, Jongseo
    • Analytical Science and Technology
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    • v.28 no.3
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    • pp.221-227
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    • 2015
  • Animal glue is a traditional material that was used widely as an adhesive in cultural artifacts, such as Buddhist paintings, dancheong (traditional multicolored paintwork on wooden buildings), mother-of-pearl inlay, and so on. Spectroscopic methods, such as infrared spectroscopy, have been used for the analysis of animal glue. However, such methods do not yield sufficient information about the constituents of the glue. Because pyrolysis/GC/MS analysis is able to estimate the components of a material through the examination of its pyrolyzed products, it is useful for the analysis of polymeric material. In this study, pyrolysis/GC/MS analysis was used to determine the chemical composition of animal glue. The appropriate conditions for analyzing animal glue were established by examining pyrolysis temperature, quantity of the sample, and the repeatability of the method. Some products of pyrolysis were identified. We also analyzed commercial gelatin and animal glue using the established method and found almost no differences in chromatograms among the samples. The results will be used as supporting data to confirm the use of animal glue in cultural artifacts and to replace traditional animal glue by commercial gelatin.

Study on the analytical method using GC-MS for the accident preparedness substances (실험실 GC-MS를 이용한 사고대비물질 분석방법 연구)

  • Kim, Kijoon;Lee, Jinseon;Lee, Suyeong;Hwang, Seungryul;Kim, Younghee;Seok, Gwangseol
    • Analytical Science and Technology
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    • v.26 no.1
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    • pp.80-85
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    • 2013
  • The sixty nine accident preparedness substances (APS) having high probability of chemical accident are controlled under the Toxic Chemicals Control Act (TCCA). Around the world, there has been a growing interest in the analysis of chemical warfare agent (CWAs). When a chemical accident occurs, it is generally required to detect and identify APS. However, the quantitative analytical data remain limited in Korea. In this study, an analytical method using GC/MS for volatile organic chemicals was established and a quantitative analysis method was studied. The calibration curve for 25 chemicals were obtained and 21 chemicals showed higher coefficient of determination ($r^2$ >0.998).

Evaluation of a Method for the Measurement of PAHs in the Ambient Atmosphere - Focusing on High Volume Sampling and GC/MS Analysis (대기 중 다환방향족탄화수소 측정방법의 성능평가 - 하이볼륨 샘플링 및 GC/MS 분석방법을 대상으로)

  • Seo, Young-Kyo;Park, Dae-Kwon;Baek, Sung-Ok
    • Journal of Environmental Health Sciences
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    • v.35 no.4
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    • pp.322-333
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    • 2009
  • In this study, a measurement method was evaluated for the determination of polycyclic aromatic hydrocarbons (PAHs) in the ambient atmosphere. PAHs were sampled by high-volume samplers, and were then analysed with a GC/MS system. Particulate PAHs were collected on $8"{\times}10"$ quartz fiber filter, while vapor phase PAHs were adsorbed on polyurethane foam (PUF). Target compounds included a total of 36 PAHs, which are known to be frequently detected in the urban atmosphere. It was not necessary to clean-up samples before samples were analyzed using GC/MS, and the overall performance of the method was tested by a variety of quality control and quality assurance schemes. It is generally known that the clean-up procedure can negatively affect the recovery of samples. Precision and accuracy was evaluated using SRM provided by US NIST, and the results were generally satisfactory and reliable. However, the GC/MS method appeared not to be adequate for 6-rings PAHs, such as coronene, due to its lower sensitivity. In addition, collection efficiencies for low molecular compounds, such as 2-rings PAHs, were poor because of the lower retention volume of the PUF adsorbent. As a result, it was concluded that the method based on high-volume sampling and GC/MS analysis can give very reliable data by simultaneous sampling of both particulate and vapor phases for 3-rings to 5-rings PAHs of environmental concern.

Analysis of Lacquer and CNSL Using Infrared Spectrometer and Pyrolysis-GC/MS (적외선분광분석과 Py-GC/MS를 이용한 옻칠 및 캐슈칠도막 분석)

  • Choi, Jaewan;Kim, Soo-Chul
    • Journal of the Korean Wood Science and Technology
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    • v.46 no.1
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    • pp.1-9
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    • 2018
  • Nowadays, synthetic resin varnish such as cashew nut shell liquid (CNSL) is being used as well as traditional lacquer. The code of ethics states that material must be identical to the original when preserving cultural heritage. Therefore, lacquer should be used. However, problem is that even experts have difficulties differentiating lacquer and CNSL as they have similar components. Therefore, this study was carried out to identify the difference between lacquer and CNSL using IR and Py-GC/MS. As a result of IR, in lacquer, $720cm^{-1}$ peak was detected and in CNSL, $750cm^{-1}$, $720cm^{-1}$ and $700cm^{-1}$ peaks were detected. The results of Py-GC/MS detect benzene compounds and alkyl chains for both varnishes. However, hexanoic acid was detected from CNSL but not lacquer. Using these analytical methods, the differences between lacquer and CNSL can be identified on the scene. This is expected to be applied to the authentic conservation and restoration of lacquerware.