• Bulletin of the Korean Chemical Society
• /
• v.28 no.4
• /
• pp.547-552
• /
• 2007

This study examined the thermal reactions of 2,4-dibromophenol (diBP), 2,6-diBP and 2,4,6-triBP. The products obtained under pyrolytic conditions were analyzed by gas chromatography/mass spectrometry (GC/MS). 2,7-dibromodibenzo-p-dioxin (diBDD) was the major compound produced from the thermal reaction of 2,4-diBP. In addition, monoBDD and triBDDs were obtained through a process of debromination and bromination, respectively. The pyrolysis of 2,6-diBP and 2,4,6-triBP produced two major brominated dioxin isomers through direct condensation and a Smiles rearrangement. The two ortho-Brs in 2,6-diBP and 2,4,6-triBP mainly led to the production of dioxins, whereas in addition to 2,7-diBDD, 2,4-diBP produced two furans as minor products, 2,8-dibromodibenzofuran (diBDF) and 2,4,8-triBDF, through the intermediate dihydroxybiphenyl (DOHB). The maximum yield of the major dioxins was obtained at 400 oC, and decomposition by debromination at 500 oC resulted in less substituted bromodioxins.

• Journal of Conservation Science
• /
• v.35 no.4
• /
• pp.363-372
• /
• 2019

Animal glue has been used as a binder in Dancheong since the Joseon dynasty. Binders play an important role in determining the physical characteristics of a painting layer. The analysis of binders can be used to identify the materials and techniques used in traditional Dancheong. Binders can be investigated using physicochemical component analyses methods such as gas chromatography/mass spectrometry, pyrolysis-gas chromatography/mass spectrometry, and fourier transform infrared spectroscopy, but the detection characteristics vary depending on the degradation properties of the pigment and binder. Therefore, cross-validation using a combination of physicochemical analysis and enzyme immunoassay is used to increase the reliability of the results. In this study, we present an enzyme-linked immunosorbent assay (ELISA) as an example of an enzyme immunoassay as a method for analyzing animal glue, a traditional binder used in Korea. The applicability of ELISA was tested using commercial animal glue, in addition to animal glue produced using a variety of extraction conditions. The animal glue was analyzed in a Noerok-additionally coated-replica sample to evaluate the possibility of analyzing the animal glue in a paint layer mixed with pigment. Based on the results, we performed an assay on the use of animal glue in the Dancheong sample of the temples of the Joseon dynasty, that are estimated to have been built in the 17^th century.

• Journal of the Korea Institute of Military Science and Technology
• /
• v.14 no.2
• /
• pp.289-298
• /
• 2011

TMAH-based Py-MS has been investigated to apply for a real-time classification of biological agents in the field. Acquiring reproducible data from mass spectrometry is a key to biological detection in the field. Nevertheless, it has been little studied on what factors could affect to the reproducibility of the TMAH-based Py-MS spectrum patterns. Given the TMAH-based Py-MS applied to the field system, several factors which could affect to the reproducible pattern of TMAH-based Py-MS spectra are needed to be examined, including changes in TMAH injection volume, growth temperature for microorganism, and number of cells collected in pyrolyzer, and implication of stabilizer used for lyophilization. This study showed that the reproducibility of the spectrum patterns was significantly hindered by changes in TMAH concentration and cell number, and stabilizer implication but not by growth temperature. Among those at low TMAH concentration(0.015m) was not observed the significant alterations of the spectrum pattern even when its injection volume was changed, yet was in different cell numbers and stabilizer implication.

• Journal of Conservation Science
• /
• v.35 no.4
• /
• pp.295-307
• /
• 2019

In the process of the conservation treatment of the glass eyes of the stone standing Maitreya of Daejosa temple, Buyeo (Treasure No. 217), a blackish material, expected to be the adhesive for fixing the glass eyes, was collected and analyzed. Infrared spectroscopy and pyrolysis/gas chromatography/mass spectrometry (pyrolysis/GC/MS) were employed to identify the organic material in the sample. The IR analysis revealed the presence of materials such as apatite or bone black. The pyrogram of the sample was similar to that of Asian lacquer, among traditional adhesives. In particular, the pyrolysis/GC/MS analysis with online methylation detected 1,2-dimethoxy-3-pentadecylbenzene, methyl 7-(2,3- dimethoxyphenyl) heptanoate, and methyl 8-(2,3-dimethoxyphenyl)octanoate. These are known to be the pyrolysis products of catechol and its oxidation product, which indicated the presence of Asian lacquer in the sample. X-ray diffraction, X-ray fluorescence, and thermal gravimetry analysis showed that the sample contained ca. 60% inorganic substances, including apatite. Radiocarbon dating of the sample suggested that the blackish material was applied between the late 13^th and early 15^th century, revealing some discrepancy with the art-historical manufacturing time of the Maitreya. From the above analysis, it was concluded that Asian lacquer and bone ash were used to attach the glass eyes by forming a thick blackish lacquer layer.

• Journal of the Korean Society of Tobacco Science
• /
• v.4 no.2
• /
• pp.63-66
• /
• 1982

Coumarin was pyrolyzed at $500^{\circ}C$ in a stream of nitrogen. The pyrolyzates of coumarin were adsorbed on the activated charcoal and then eluded by carbon disulfide. The eluted pyrolyzates were identified using a gas chromatography/mass spectrometry. Benzene, toluene, phenylacetylene, styrene, benzofuran and naphthalene were detected from the pyrolyzates of coumarin on the basis of their mass spectra. The pyrolytic mechanism of coumarin was also discussed.

• Bulletin of the Korean Chemical Society
• /
• v.35 no.7
• /
• pp.2057-2064
• /
• 2014

Thermochemical sulfate reduction (TSR) was conducted in autoclave on the system of crude oil and $MgSO_4$ at different temperatures. Gas chromatography pulsed flame photometric detector (GC-PFPD) was used to detected the composition of organic sulfur compounds in oil phase products. The results of the analysis indicate that with increased temperature, the contents of organic sulfur compounds with high molecular weight and thermal stability, such as benzothiophenes and dibenzothiophenes, gradually became dominated. In order to gain greater insight into the formation and distribution of organic sulphur compounds from TSR, positive ion electrospray Fourier transform ion cyclotron resonance mass spectrometry (FT-ICR MS) was used in detecting the detailed elemental composition and distribution of them. The mass spectra showed that the mass range of sulfur compounds was 200-550 Da. Four sulfur class species, $S_1$, $N_1S_1$, $O_1S_1$ and $O_2S_1$, were assigned in the positive-ion spectrum. Among the identified sulfur compounds, the $S_1$ class species was dominant. The most abundant $S_1$ class species increase associated with the DBE value and carbon number increasing which also indicates the evolution of organic sulfur compounds in TSR is from the labile series to the stable one. In pure blank pyrolysis experiments with crude oil cracking without TSR, different composition and distribution of organic sulfur compounds in oil phase products were seen from mass spectra in order to evaluate their pyrolysis behaviors without $MgSO_4$. FT-IR and XRD were used in analyzing the products of solid phases. Two distinct crystallographic phases MgO and $MgSO_4$ are found to coexist in the products which demonstrated the transformation of inorganic sulfur compounds into organosulfur compounds exist in TSR.

• Applied Chemistry for Engineering
• /
• v.29 no.2
• /
• pp.248-251
• /
• 2018

Catalytic pyrolysis of the waste paper cup containing coffee residual (WPCCCR) was performed using a fixed bed reactor and pyrolyzer-gas chromatography/mass spectrometry (Py-GC/MS). Non-catalytic pyrolysis of WPCCCR produced a large amount of oil together with gas and char. The use of both HZSM-5 and HY decreased the yields of oil and increased the yield of gas due to the additional catalytic cracking. Owing to the acidic catalytic properties of HZSM-5 and HY, catalytic Py-GC/MS analysis of WPCCCR increased the selectivity to aromatic hydrocarbons in product oil. Owing to properties of HZSM-5 having a stronger acidity and medium pore size, the catalytic pyrolysis of WPCCR over HZSM-5 produced much larger amounts of aromatic hydrocarbons than that of using HY.

• Proceedings of the Korea Technical Association of the Pulp and Paper Industry Conference
• /
• 2006.06a
• /
• pp.173-176
• /
• 2006

Pyrolysis-gas chromatography (Py-GC) in the presence of organic alkali of tetrabutylammonium hydroxide (TBAH) was applied to characterize the polyphenol fragments with a carbonyl group causing different magnitude of photo-yellowing in chemithermomechanical pulp (CTMP) papers. Two different origin of CTMP papers prepared from different individuals of Eucalyptus globulus trees showing high and low yellowing after photo-irradiation was compared before photo-irradiation. As a result, 7 peaks assigned to a series of phenol compounds with a carbonyl group, derived mainly from lignin, gave significant amount of phenol compounds with a carbonyl group for the paper sample of latent high yellowing, i.e., butoxy-and syringaldehyde, butoxy-and syringylacetone, butoxy-acetoguaiacone, butoxy-acetosyringone, butoxy-acetoethylsyringone, 3-methoxy-4-butoxy butyl ester, and 3,5-dimethoxy-4-butoxy butyl ester, using Py-GC/mass spectrometry (MS). The Py-GC method combined with TBAH successfully characterized polyphenol fragments with a carbonyl group causing differ high photo-yellowing in CTMP papers using a microgram order of samples.

• Conservation Science in Museum
• /
• v.30
• /
• pp.47-70
• /
• 2023

In 2019, the first excavation survey was conducted at the Temple Site No. 4 of Yaksugok Vally in Namsan Mountain, Gyeongju to determine the original location of the headless stone Buddha statue and the structure of the temple site. The survey excavated a stone Buddha head that was confirmed in a comparative analysis to be petrologically and mineralogically identical to a headless stone seated Buddha statue found derelict nearby. Traces of gold leaf and black adhesive were found on a portion of the right side of the face of the Buddha head buried in the ground. Since it is exceedingly rare for lacquer and gilding techniques to have been applied to a large stone Buddha statue without a base layer, this study examines the gilding techniques of the time by analyzing the characteristics of the materials used. In this process, the structure of the gold foil was observed through analytical microscopy and scanning electron microscopy with energy dispersive X-ray spectrometry, and the gold (Au) component was identified. As a result of analyzing the black adhesive using pyrolysis-gas chromatograph/mass spectrometry (pyrolysis-GC/MS), pyrolysis compounds such as hydrocarbons, fatty acids, catechol, and catechol oxidation products were detected. This was identical to the characteristics identified upon analyzing lacquer collected from species of lacquer tree whose main component is urushiol. Therefore, it was confirmed that the stone Buddha head excavated from the Temple Site No. 4 of Yaksugok Valley was separated from a nearby stone seated Buddha statue, and that the gold foil was attached using lacquer sap collected from lacquer trees, which grow in Korea, China, and Japan.

• Journal of Ecology and Environment
• /
• v.46 no.4
• /
• pp.282-291
• /
• 2022

Background: The Arctic permafrost stores enormous amount of carbon (C), about one third of global C stocks. However, drastically increasing temperature in the Arctic makes the stable frozen C stock vulnerable to microbial decomposition. The released carbon dioxide from permafrost can cause accelerating C feedback to the atmosphere. Soil organic matter (SOM) composition would be the basic information to project the trajectory of C under rapidly changing climate. However, not many studies on SOM characterization have been done compared to quantification of SOM stocks. Thus, the purpose of our study is to determine soil properties and molecular compositions of SOM in four different Arctic regions. We collected soils in different soil layers from 1) Cambridge Bay, Canada, 2) Council, Alaska, USA, 3) Svalbard, Norway, and 4) Zackenberg, Greenland. The basic soil properties were measured, and the molecular composition of SOM was analyzed through pyrolysis-gas chromatography/mass spectrometry (py-GC/MS). Results: The Oi layer of soil in Council, Alaska showed the lowest soil pH and the highest electrical conductivity (EC) and SOM content. All soils in each site showed increasing pH and decreasing SOC and EC values with soil depth. Since the Council site was moist acidic tundra compared to other three dry tundra sites, soil properties were distinct from the others: high SOM and EC, and low pH. Through the py-GC/MS analysis, a total of 117 pyrolysis products were detected from 32 soil samples of four different Arctic soils. The first two-axis of the PCA explained 38% of sample variation. While short- and mid-hydrocarbons were associated with mineral layers, lignins and polysaccharides were linked to organic layers of Alaska and Cambridge Bay soil. Conclusions: We conclude that the py-GC/MS results separated soil samples mainly based on the origin of SOM (plants- or microbially-derived). This molecular characteristics of SOM can play a role of controlling SOM degradation to warming. Thus, it should be further investigated how the SOM molecular characteristics have impacts on SOM dynamics through additional laboratory incubation studies and microbial decomposition measurements in the field.