• Title/Summary/Keyword: analytical pyrolysis

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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.

Fabrication and Characterization of Macro/Mesoporous SiC Ceramics from SiO2 Templates (실리카 주형을 이용한 메크로/메조다공성 탄화규소 세라믹의 제조와 비교특성)

  • ;Hao Wang
    • Journal of the Korean Ceramic Society
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    • v.41 no.7
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    • pp.528-533
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    • 2004
  • Macroporous SiC with pore size 84∼658 nm and mesoporous SiC with pore size 15∼65 nm were respectively prepared by infiltrating low viscosity preceramic polymer solutions into the various sacrificial templates obtained by natural sedimentation or centrifuge of 20∼700 nm silica sol, which were subsequently etched off with HF after pyrolysis at 1000∼140$0^{\circ}C$ in an argon atmosphere. Three-dimensionally long range ordered macroporous SiC ceramics derived from polymethylsilane (PMS) showed surface area 584.64$m^2$g$^{-1}$ when prepared with 112nm silica sol and at 140$0^{\circ}C$, whereas mesoporous SiC from polycarbosilane (PCS) exhibited the highest surface area 619.4 $m^2$g$^{-1}$ with random pore array when prepared with 20-30 nm silica sol and at 100$0^{\circ}C$. Finally, tile pore characteristics of porous SiC on the types of silica sol, polymers and pyrolytic conditions were interpreted with the analytical results of SEM, TEM, and BET instruments.

Chemical Features of Solid Residues Obtained from Supercritical Water Treatment of Populus alba×glandulosa (현사시나무 목분의 초임계수 처리 공정으로부터 유래한 미분해 고형성분의 화학적 특성)

  • Kim, Kwang Ho;Eom, In Yong;Lee, Soo Min;Lee, Oh Kyu;Meier, D.;Choi, Joon-Weon
    • Journal of the Korean Wood Science and Technology
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    • v.37 no.4
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    • pp.372-380
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    • 2009
  • After supercritical water treatment of poplar wood meals (passed through 60 mesh) for 60s between 325 and $425^{\circ}C$ at the fixed pressure at $220{\pm}10atm$, some solid residues were present in the degradation products. They mainly consisted of chemically modified lignin and fibrous materials. Glucose and xylose were identified as main sugar components of fibrous materials, and the highest ratio of glucose/xylose was achieved at the highest reaction temperature. As reaction temperature was elevated, the portion of fibrous materials decreased in the solid residues, while lignin was further accumulated. The H : G : S ratio of lignin in solid residues was estimated by analytical pyrolysis. Irrespective of reaction temperatures, the H:G:S ratios were not significantly changed in the lignin in solid residues. Compared to poplar milled wood lignin (MWL), it was remarkable that H type monomers were further lowered, while portion of S type monomers increased. The amount of G type monomers were relative stable. In presence of HCl catalyst, lowering H type as well as enhancing S type was further distinguishable. According to the result of nitrobenzene oxidation (NBO), ca. 265 mg of vanillin and syringaldehyde was yielded from poplar MWL as main products. However, remarkably reduced amount of NBO products were determined from solid residues by raising operating temperature as well as by the addition of HCl catalyst. These results strongly indicate that $\beta$-O-4 linkage could be easily cleaved during supercritical water treatment, so that the lignins in the solid residues seem to be condensed phenol polymers, which are mainly formed by carbon-carbon linkages rather than $\beta$-O-4 linkage.

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.

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.