• Title, Summary, Keyword: py-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.

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.

Measurement of Degree of Hydrolysis of a PA66/GF Composite using a py-GC/MS analysis

  • Lee, Jong-Young;Kim, Kwang-Jea
    • Elastomers and Composites
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    • v.52 no.1
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    • pp.59-68
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    • 2017
  • The effect on the hydrolysis resistance properties by the addition of maleic anhydride grafted EMDM (MA-g-EPDM) and PP (MA-g-PP) to a PA66/GF composite was investigated with respect to the mechanical properties, thermal properties, and morphology. The degree of hydrolysis of the PA66/GF composite was measured using py-GC/MS analysis. When compared to the PA66/GFcomposite in MEG/water solution, the composites where MA-g-EPDM and MA-g-PP were added to PA66/GF showed a higher degree of hydrolysis resistance, impact strength, and thermal properties, whereas their tensile strength, tensile modulus, flexural strength and flexural modulus decreased. As immersion time in the solution increases, the rate of tensile strength drop of the MA-g-PP added composite appeared lower than that of the PA66/MA-g-EPDM/GF and PA66/GF composites. The py-GC/MS analysis confirmed the formation of PA66 hydrolysis reaction by products such as carboxylic acid and alkylamine with increasing immersion time.

Building Calibration Curve for Py-GC/MS Analysis of SBR/BR Blend Rubber Compounds

  • Chae, Eunji;Choi, Sung-Seen
    • Elastomers and Composites
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    • v.55 no.4
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    • pp.281-288
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    • 2020
  • A calibration curve is needed to determine the SBR and BR blend ratio of SBR/BR blend rubber compounds using pyrolysis-gas chromatography/mass chromatography (Py-GC/MS) or Py-GC. In general, a calibration curve is obtained using reference SBR/BR vulcanizates with various blend ratios. In this study, the calibration curves were obtained using reference samples made of rubber solutions and were compared to those plotted using the reference SBR/BR vulcanizates. Calibration curves using variations of 1,3-butadiene/styrene, 4-vinylcyclohexene (VCH)/styrene, 2-phenylpropene (PhP)/butadiene, PhP/VCH, 4-phenylcyclohexene (PhCH)/butadiene, and PhCH/VCH ratios with the BR content were examined for the suitability. We found that the calibration curves obtained using the mixed rubber solution references (1,3-butadiene/styrene and PhP/butadiene) could replace those constructed using the reference SBR/BR vulcanizates. The calibration curves of 1,3-butadiene/styrene and PhP/butadiene obtained using the raw references can be used for the determination of the SBR/BR blend ratios by applying some correction factors.

Identification of Marker Compounds for Discriminating between Embryogenic and Nonembryogenic Calluses of Higher Plants Using Pyrolysis Gas Chromatography Mass Spectrometry and Genetic Programming

  • Kim Suk-Weon;Ban Sung-Hee;Yoo Ook-Joon;Liu Jang-Ryol
    • Biotechnology and Bioprocess Engineering:BBE
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    • v.11 no.1
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    • pp.38-42
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    • 2006
  • When whole cells are subjected to pyrolysis gas chromatography/mass spectrometry (Py-GC/MS) analysis, it provides biochemical profiles containing overlapping signals of the majority of compounds. To determine marker compounds that discriminate embryogenic calluses from nonembryogenic calluses, samples of embryogenic and nonembryogenic calluses of five higher plant species were subjected to Py-GC/MS. Genetic programming of Py-GC/MS data was able to discriminate embryogenic calluses from nonembryogenic calluses. The content ratio of 5-meyhyl-2-furancarboxaldehyde and 5-(hydroxymethyl)-2-furancarboxaldehyde was greater in nonembryogenic calluses than in embryogenic calluses. However, the content ratio of phenol, p-cresol, and $^1H-indole$ in embryogenic calluses was 1.2 to 2.4 times greater than the ratio in nonembryogenic calluses. These pyrolysates seem to be derived from the components of the cell walls, which suggests that differences in cell wall components or changes in the architecture of the cell wall playa crucial role in determining the embryogenic competence of calluses.

Organic Material Analysis of a Lacquered Wooden Sheath of Long Sword with Ring Pommel Excavated in Imdang Ancient Tomb (경산 임당고분 출토 철제 고리자루칼 칠의 유기물 분석)

  • Park, Jongseo;Cho, Ha-nui;Lee, Jae-sung
    • Journal of Conservation Science
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    • v.34 no.5
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    • pp.369-377
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    • 2018
  • In order to examine the constituents and weathered state of a lacquer specimen, analysis of the organic materials was conducted using py/GC/MS(pyrolysis-gas chromatography-mass spectrometry). The samples were obtained from the lacquered wooden sheath of a long ring-pommel sword excavated in the Imdang No.1 ancient tomb constructed around the Proto-Three Kingdoms period. In direct py/GC/MS, the sample and the dried Asian lacquer showed similar chromatograms, while the characteristic compounds of Asian lacquer such as 1,2-dimethoxy-3-pentadecylbenzene were observed in THM(thermally assisted hydrolysis and methylation)-py/GC/MS. In addition, compounds like dimethyl nonanedioate, which presumably originated from drying oil, were also detected. Furthermore, the detection of oxidized catechols in considerable amount indicated that the degradation of lacquer is estimated to result from the oxidation of urushiol. Therefore, it is suggested that the lacquered wooden sheath was prepared using Asian lacquer and drying oil, and that the lacquer layer was considerably oxidized over the long burial time.

Analysis of Poly(Ethylene-co-Vinyl Acetate) Using Off-line Pyrolysis

  • Choi, Sung-Seen;Kim, Eunha
    • Elastomers and Composites
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    • v.51 no.1
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    • pp.63-67
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    • 2016
  • Poly(ethylene-co-vinyl acetate) (EVA) was pyrolyzed to eliminate acetic acid of VA unit using off-line pyrolysis, and the deacetylated EVA was analyzed infrared spectroscopy (IR) and pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS). EVA film for deacetylation was prepared by solution casting on aluminum foil and it was pyrolyzed at low temperature of $300^{\circ}C$ in the off-line pyrolysis apparatus. After deacetylation, carbon-carbon double bond (C=C) was formed by 1,2-elimination of the VA unit in the EVA backbone. Most of C=C bonds were trans-1,4-unit and 1,2-unit was also observed. Presence of the 1,2-unit in deacetylated EVA indicates that terminal or branch VA units exist in the raw EVA. Py-GC/MS chromatogram of deacetylated EVA displayed much smaller acetic acid and much more abundant other pyrolysis products than that of raw EVA, which means that the pyrolysis efficiency and separation condition were improved.

Catalytic Pyrolysis of Waste Polyethylene Terephthalate over Waste Concrete

  • Lim, Sejeong;Kim, Young-Min
    • Applied Chemistry for Engineering
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    • v.30 no.6
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    • pp.707-711
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    • 2019
  • The feasibility of waste concrete as a catalyst for the effective pyrolysis of polyethylene terephthalate (PET) was examined using thermogravimetric (TG) and pyrolyzer-gas chromatography/mass spectrometry (Py-GC/MS) analyses. TG analysis results indicated that the maximum decomposition temperature of PET is not altered by the use of waste concrete, showing similar values (407 ℃ and 408 ℃ at 5 ℃/min). Meanwhile, the volatile product distribution data obtained from the Py-GC/MS analysis revealed that the use of waste concrete promoted the deoxygenation reaction via converting the oxygen containing products such as benzoic acids, benzoates, and terephthalates to valuable deoxygenated aromatic hydrocarbons including benzene, toluene, ethylbenzene, and styrene. This suggests that the waste concrete can be used as a potential catalyst for the production of valuable aromatic hydrocarbons from PET pyrolysis.

Confirming Animal Glue in Dancheong Sample by Pyrolysis/GC/MS (열분해/GC/MS에 의한 재현 단청 시편에서 아교의 확인)

  • Park, Jong Seo;Kim, Mi Jeong;Kim, Soon Kwan
    • Journal of Conservation Science
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    • v.32 no.1
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    • pp.21-32
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    • 2016
  • Animal glue is a traditional material used extensively as adhesive and binder in mother-of-pearl, wooden structure, traditional painting, etc. Analysis of animal glue is usually performed with IR(infrared spectroscopy) based on the IR absorption of functional group. But, it has a limitation in confirming animal glue when a sample consists of several materials because of overlapping of the absorption band. Py/GC/MS(pyrolysis/gas chromatography/mass spectrometry) is a useful tool in analyzing the constituent of polymeric materials like animal glue by identifying their pyrolysate with very small amount of sample. In this study, confirmation of animal glue in a Dancheong sample was tried with this method. Characteristic pyrolytic compounds of animal glue and tung oil used in Dancheong were identified. Dancheong sample painted with Noerok as a coloring material, animal glue and tung oil was prepared and it was possible to find characteristic peaks of animal glue after thermal degradation and artificial weathering experiment. From this, we found that animal glue can be detected using py/GC/MS in cultural heritage samples consisting of several materials and in different condition. IR was also tried to analyze Dancheong sample and the results were compared with those of py/GC/MS for the detection of animal glue.

Identification of the Derivated Species from Traditional Coating Films (전통 칠 유래 성분의 확인)

  • Shin, Jeoung Hwa;Ahn, Yun Gyong
    • The Korean Journal of Community Living Science
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    • v.24 no.2
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    • pp.243-249
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    • 2013
  • Identification of coating film species from ancient coating materials is needed to maintaine their surfaces without loss of their original beauty for a long time and understand the historical background of manufacturing techniques. A pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS) was applied to identify the origine of films in ancient coating materials. The pyrolysis products, which reflect the source from which they originate were detected distinctively at $500^{\circ}C$. This is a rapid technique that does not require large amounts of sample or any sample preparation. Sesquiterpenes are a class of terpenes that consist of three isoprene units were identified as cadienes, selinenes, cubebenes from the raw material of dendropanax morbifera. On the other hand, alkanes(tetra~heptadecanes), alkenes (tri~heptadecenes), allkyphenols, catechols and fatty acids were detected from the raw material of the lacquer film. Based on these results, the origine of historic coatings artifacts was identified using py-GC/MS by comparison with their pyrolysis products.