• Title/Summary/Keyword: Py-MS

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Characterization of Poly(methyl methacrylate)-tin (IV) Chloride Blend by TG-DTG-DTA, IR and Pyrolysis-GC-MS Techniques

  • Arshad, Muhammad;Masud, Khalid;Arif, Muhammad;Rehman, Saeed-Ur;Saeed, Aamer;Zaidi, Jamshed Hussain
    • Bulletin of the Korean Chemical Society
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    • v.32 no.9
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    • pp.3295-3305
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    • 2011
  • Thermal behavior of poly (methyl methacrylate) was analyzed in the presence of tin (IV) chloride. Five different proportions - polymer to additive - were selected for casting films from common solvent. TG, DTG and DTA were employed to monitor thermal degradation of the systems. IR and py-GC-MS helped identify the decomposition products. The blends start degrading at a temperature lower than that of the neat polymer and higher than that of the pure additive. Complex formation between tin of additive and carbonyl oxygen (pendent groups of MMA units) was noticed in the films soon after the mixing of the components in the blends. The samples were also heated at three different temperatures to determine the composition of residues left after the expulsion of volatiles. The polymer, blends and additive exhibited a one step, two-step and three-step degradation, respectively. $T_0$ is highest for the polymer, lowest for the additive and is either $60^{\circ}C$ or $70^{\circ}C$ for the blends. The amount of residue increases down the series [moving from blend-1 (minimum additive concentration) to blend-5 (maximum additive concentration)]. For blend-1, it is 7% of the original mass whereas it is 16% for blend-5. $T_{max}$ also goes up as the concentration of additive in the blends is elevated. The complexation appears to be the cause of observed stabilization. Some new products of degradation were noted apart from those reported earlier. These included methanol, isobutyric acid, acid chloride, etc. Molecular-level mixing of the constituents and "positioning effect" of the additive may have brought about the formation of new compounds. Routes are proposed for the appearance of these substances. Horizontal burning tests were also conducted on polymer and blends and the results are discussed. Activation energies and reaction orders were calculated. Activation energy is highest for the polymer, i.e., 138.9 Kcal/mol while the range for blends is from 51 to 39 Kcal/mol. Stability zones are highlighted for the blends. The interaction between the blended parts seems to be chemical in nature.

Petrogenesis and Metamorphism of Charnockite of Eastern Jirisan Area (지리산 동부 지역에 분포하는 차노카이트의 변성작용과 성인에 관한 연구)

  • 김동연;송용선;박계헌
    • The Journal of the Petrological Society of Korea
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    • v.11 no.3_4
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    • pp.138-156
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    • 2002
  • Precambrian metamorphic rocks of southwest Sobaeksan massif consist of mainly granitic gneiss, porphyroblastic gneiss and quartzofeldspathic gneiss. The orthopyroxene-bearing rocks(charnockites) are found in the west of Hadong-Sancheong anorthosite complex. The charnockites are 3km wide, 12km long and divided into massive and foliated types based on their texture. The compositions of charnockites are comparable to granodiorite to adamellite and subalkaline. Variations in major and trace elemental abundances show typical magmatic differentiation trends. The geochemical data plotted on tectonic discrimination diagrams reveal that these charnockites were formed in the active tectonic environment. The massive and folidated charnockites are mainly composed of plagioclase, orthopyroxene, microcline, quartz and disseminated garnet. Camels generally show characteristic zonal textures with decreasing $X_{alm}$(0.74~0.83), $X_{Py}$ (0.07~0.12) and $X_{Mg}$ (0.12~0.08) and increasing $X_{grs}$(0.03~0.15) from core to rim. Metamorphic temperature and pressure of the charnockites estimated from orthopyroxene-garnet-plagioclase-quartz assemblages show wide range of variation of $600~900^{\circ}C$ and 2.5~7.5 kbar respectively. The results of P-T estimates indicate an anticlockwise P-T evolution path.

Comparison of Pyrolysis Patterns of Different Tobacco Leaves by Double-Shot Pyrolysis-GC/MSD Method

  • Lee, Chang-Gook;Lee, Jae-Gon;Jang, Hee-Jin;Kwon, Young-Ju;Lee, Jang-Mi;Kwag, Jae-Jin;Kim, Soo-Ho;Sung, Yong-Joo;Shin, Chang-Ho;Kim, Kun-Soo;Rhee, Moon-Soo
    • Journal of the Korean Society of Tobacco Science
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    • v.30 no.2
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    • pp.94-102
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    • 2008
  • In this paper, we describe our study on the characterization of tobacco leaves by their pyrolysis patterns. Two kinds of tobacco leaves were pyrolyzed and analyzed by Double-Shot Pyrolysis-Gas Chromatography/Mass Spectroscopy (Py-GC/MS) methods. Three grades of Korean flue-cured tobacco leafsuch as B1O, AB3O, CD3L and burley tobacco leaves such as B1T, AB3T, CD3W were pyrolyzed with six discrete but stepwise heating temperature ranges, those are from 100$^{\circ}C$ to 150$^{\circ}C$, 150$^{\circ}C$ to 200$^{\circ}C$, 200$^{\circ}C$ to 250$^{\circ}C$, 250$^{\circ}C$ to 300$^{\circ}C$, 300$^{\circ}C$ to 350$^{\circ}C$ and finally from 350$^{\circ}C$ to 400$^{\circ}C$. Using the resultant 52 pyrolytic components identified in the programs as components, principal component analysis (PCA) showed statistical classification between flue-cured and burley tobacco lamina. Among six pyrolysis temperature ranges, the best discrimination was achieved at the temperature range from 250$^{\circ}C$ to 300$^{\circ}C$ and from 300$^{\circ}C$ to 350$^{\circ}C$.

A Study on the Effect of Alleolopathy of Vitex negundo var. incisa Leaves Extracts (좀목형 엽 추출물의 Allelopathy에 관한 연구)

  • 서병수;문성필;손정훈
    • Korean Journal of Environment and Ecology
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    • v.15 no.2
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    • pp.173-185
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    • 2001
  • 마편초과의 좀목형 엽에 함유된 물질의 allelopathy 효과를 구명하기 위해 수용성 엽 추출액, 메탄올 엽 추출액, 엽 분말과 토양과의 혼화된 pot에 각각 상치, 이탈이란라이그라스, 개솔새, 억새 종자를 발아실험하여 발아억제물질을 분석한 결과는다음과 같다. 1. 좀목형 엽 분말을 증류수에 각각 24, 48, 72 시간 침지 후 추출물에 상치, 이탈리안라이그라스, 개솔개, 억새 종자를 파종한 후의 발아율은 각 처리구마다 대조구마다 높은 발아억제를 보였고, 48시간 침지시에는 각각 26.9%, 58.8%, 6.6%, 22.2%의 발아율을 보여 강한 발아억제현상르 보였다. 2. 좀목형 엽 분말을 메탄올 75%에 24, 48시간 침지 후 추출물에 이탈리아라이그사스, 개솔새, 억새 종자를 파종한 후의 발아율은 48시간 추출액때 각각 33.3%, 15.4%, 7.7%를 보여 48시간 수용성 추출액과 24시간 메탄올 추출액보다 강한 발아억제효과가 있었다. 3. 좀목형 엽 분말과 Vermiculite를 1: 99.5: 95, 10:90, 20:80(w/w)으로 구분한 pot에 공시수종을 파종한 결과 엽 분말의 비율이 높을수록 발아억제효과가 컸으며, 엽 분말이 20%인 경우 발아된 부분의 건중량의 비율은 실험구와 대조구간에 비교한 발아율의 비율보다 훨씬 낮아 생장억제효과가 있는 것으로 나타났다. 4. Column chromatography의 TLC를 이용하여 최종 7 fraction을 찾고 생물검정 결과, 5, 6번 fraction에 강한 활성을 나타냈다. 5. UV 와 IR분광분석 결과 UV 분광분석은 256 nm과 336nm에서 흡수 최대를 나타내었으며, 이들은 시르시트시약을 사용하여 검토한 결과 7위에 에테르 결합한 전형적인 플라본류로 추정되었고, IR 분광분석 결과 지방족에 에테르결합이 존재하는 것으로 생각되었다. 6. Py-GC-MS 분석으로부터 5, 6 fraction의 경우 플라본류에 1개의 당이 결합한 배당체 구조이고 B환의 경우 1개 또는 2개 이상의 페놀성 수산기의 존재가 예상되었다.

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Scientific Study on Clepsydra of Changgyeonggung Palace, National Treasure for Diagnosis on State of Conservation (국보 창경궁 자격루 누기의 보존상태 진단을 위한 과학적 조사)

  • YOU Harim;LEE Jaesung;YU Jia;JO Hanui;PARK Younghwan;RYU Dongwan
    • Korean Journal of Heritage: History & Science
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    • v.56 no.3
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    • pp.138-156
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    • 2023
  • Some of the metal cultural heritage that make up a considerable proportion of Korea's cultural heritage have been installed and displayed outdoors due to their own functions, roles, and scale. Therefore, more diverse and complex damages can occur outdoors than they are in a stable environment. Therefore, it is necessary to combine accurate diagnosis and systematic survey methods in order to utilize basic data obtained from research results as data for the long-term and continuous conservation management as well as to do the research to diagnose the conservation status of outdoor cultural heritage. The clepsydra(hereinafter referred to as Jagyeongnu) of Changgyeonggung Palace, the National Treasure has been installed and displayed outdoors since it was manufactured. Though regular conservation and maintenance of the Jagyeongnu have been carried out, damage still occurred. Therefore, the scientific research on Jagyeongnu to diagnose the state of conservation was conducted prior to the full-scale conservation treatment. First, the state of conservation was investigated with an examination of basic data, macroscopic inspections and past records of repair history according to the purpose of the research. More detailed examinations were also conducted through the 3D scan, surface pattern investigation, and color difference analysis, and the analysis on materials and contaminants were conducted through P-XRF, FT-IR, and Py-GC/MS. The scientific research reveals that squalane and silicone oil have been applied in the past for conservation treatment and directly exposed to outdoor environmental factors, which caused damage to Jagyeongnu and contaminants such as dust adhered thickly to its surface, accelerating severe damage. A greater incidence of damage was found around the part with relatively high exposure effect, which corresponded with the tendency identified by grouping color difference data. As a result of integrating various research methodologies to diagnose the state of conservation and secure basic data, the causes and types of damage were identified. Furthermore, the process of obtaining digital data to be utilized in various ways, and the color difference analysis presenting visible damage as scientific data and identifying the tendency of damage patterns were confirmed to have been effective.

A case study of verifying a suicide by carbon monoxide intoxication committed by burning an ignition charcoal briquette (착화탄 연소에 의한 일산화탄소 중독사에서 자살입증에 관한 사례연구)

  • Sung, Tae-myung;Jo, Ju-ik;Ahn, Phil-sang
    • Analytical Science and Technology
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    • v.28 no.6
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    • pp.398-408
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    • 2015
  • Carbon monoxide (CO) intoxication, arising from CO from an ignited charcoal briquette (ICB), is a popular means of committing suicide in Korea. Most CO intoxications are related to suicide attempts; however, the possibility of a homicide disguised as a suicide cannot be ruled out. Therefore, forensic investigation of the deceased and the crime scene is crucial to confirm that the deceased committed suicide. Detection of the components of an ICB on the objects suspected of being contacted by the deceased, such as the hands, nostrils, and doorknobs, is essential for linking the crime scene to the victim in the case of suicides by ignited ICBs. The traces from an ICB were analyzed by investigating the morphological characteristics and obtaining elemental compositions. The ICBs were completely different from blackened wood, as detected by discriminant analysis with the elements of carbon and oxygen. We analyzed one case of CO intoxication to demonstrate an excellent procedure for verifying whether a suicide occurred with an ICB. We employed SEM-EDX for the analysis of an ICB, microscope-FT/IR and pyrolysis-GC/MS for a partly burnt resin-type substance, GC/MS for diphenhydramine (a sleeping drug), and GC/TCD for the CO-Hb level. We detected traces of an ICB on the hands, nostrils, and doorknobs, which were all discriminated into an ICB group. Detection of ICB traces from the nostrils could indicate that the deceased started the fire themselves to commit suicide. The partially burnt black material was analyzed as an acrylronitrilestyrene polymer, which is normally used to make bags for carrying or wrapping and could be assumed to have been used to transport the ICB. Diphenhydramine, a sleeping drug, was detected at a level of 2.3 mg/L in the blood, which was lower than that in fatal cases (8-31 mg/L; mean 16 mg/L). A CO-Hb level of 79% was found in the blood, which means that the cause of death was CO intoxication. The steps shown here could represent an ideal method for reaching a verdict of suicide by CO intoxication produced by burning an ICB in a sealed room or a car.

A Study on the analysis method and composition characteristics of organic materials in the pottery excavated at the palace site in Yongjangseong Fortress, Jindo (진도 용장성 왕궁지 출토 도기호 내부 유기물의 분석법과 성분 특성 연구)

  • YUN Eunyoung;YU Jia;KIM Kyuho
    • Korean Journal of Heritage: History & Science
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    • v.56 no.3
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    • pp.158-171
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    • 2023
  • Pottery filled with organic materials was excavated from the G-2 building site of Yongjangseong Fortress, Jingo, a relic of the Goryeo Dynasty. In this study, the characteristics of organic material were confirmed by a scientific analysis of organic material in pottery found at the palace in Yongjangseong, Jindo. In addition, it was intended to review the analysis method to identify the natural resin and to secure characteristic components(biomarkers) for each natural resin and use them as basic data in the future. The organic materials in the pottery were analyzed using attenuated total reflectance Fourier-transformed infrared spectroscopy(ATR-FTIR) and gas chromatography mass spectrometry(GC-MS). The infrared spectral characteristics were estimated to be natural resin, and biomarkers of organic materials were identified as sesquiterpene-based compounds(C15H24, MW 204) and derivatives. The lacquer(T.vemicifluum) is composed mainly of alkenes, alkanes, and catechol. Pine resin(P.densiflora), on the other hand, is primarily composed of diterpenoid(abietic acid, pimaric acid) and Whangchil(yellow lacquer) is identified to have sesquiterpenes(such as selinene, muurolene, calamenene) as its main components. So, the organic material in the pottery can be identified as Whangchil by comparing their compounds with modern resin materials from Dendropanax. morbifera that correspond with the results. Whangchil, which is exuded from the Dendropanax. morbifera, has been used as a natural coating materials since ancient times, and it has been confirmed that the characteristic components are well preserved even 700 years later. It can be assumed that the interior Whangchil was stored not for use as a coating, but rather for ritual purposes when the building was constructed, because the pottery was found near the cornerstone. Furthermore, based on simplified sample preparation using pyrolysis-gas chromatography mass spectrometry(Py-GC-MS), the thermal decomposition products were found to be similar to the characteristic components, suggesting that this method can be applied to the identification of natural resins used in historic artifacts.