• 제목/요약/키워드: TG-DTG

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TG/DTG 방법에 의한 EPDM/IIR 고무 블렌드의 열분석 (Thermal Characterization of an EPDM/IIR Rubber Blend using TG/DTG Anylsis)

  • 안원술
    • Elastomers and Composites
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    • 제42권1호
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    • pp.55-58
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    • 2007
  • TG/DTG 열분석법을 이용하여 EPDM/IIR 고무 블렌드의 열적 성질을 각각의 EPDM 및 IIR 샘플과 비교하여 시험하고 그 들 상호간의 상용성을 연구하였다. 실험에서 EPDM/IIR 고무 블렌드 샘플의 TGA 열분석곡선은 EPDM 및 IIR의 고유한 열분해 특성을 동시에 반영하는 모습을 나타내었다. 각각의 샘플에 대한 DTG 곡선을 구하여 본 결과, 블렌드의 DTG 곡선은 EPDM과 IIR 의 DTG peak 특성을 각각 나타내는 두 개의 peak로 분리되어 나타났으며, 특히 IIR의 특성 peak는 원래 IIR peak보다 약 $25\;^{\circ}C$ 정도 고온으로 이동하여 나타난 반면 EPDM의 특성 peak는 약 $15\;^{\circ}C$ 정도 저온으로 이동하여 나타났다. 이러한 결과로부터 EPDM이 IIR에 비해 상대적으로 열적 안정성이 더 큰 것으로 생각되었으며, 또한 EPDM과 IIR의 블렌드는 부분적으로 상용성이 있는 것으로 판단되었다. 또한 미리 결정된 EPDM/IIR 블렌드의 조성비에 따른 DTG 곡선과의 관계를 미리 준비해 두게 되면, 본 실험에서와 같이 비교적 간단한 TGA 실험을 통하여 미지의 EPDM/IIR 블렌드에 대한 조성비도 다른 고무 블렌드에서와 마찬가지로 정량적인 정보를 얻어 낼 수 있었다.

DTG 분석법을 활용한 슬래그류 비탄산염 재료의 CO2 정량 측정방법 연구 (A Study on the Method for Quantifying CO2 Contents in Decarbonated Slag Materials by Differential Thermal Gravimetric Analysis)

  • 최재원;유병노;추용식;한민철
    • 한국건설순환자원학회논문집
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    • 제12권1호
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    • pp.8-16
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    • 2024
  • 포틀랜드 시멘트, 철강 산업 등에서 원료로 사용되는 석회석(CaCO3, calcium carbonate)은 고온에서 탈탄산 분해 반응에 의해 CO2를 배출한다. 석회석 사용에 의한 CO2 배출을 저감하기 위해 CO2 배출의 원인이 되는 carbonate 광물을 함유하지 않거나 함유량이 적으면서도 CaO를 함유한 산업부산물로 석회석을 대체하려는 기술이 제안되었다. 이들 산업부산물에 함유된 CO2를 정량 측정하는 방법으로 Loss of Ignition(LOI), Thermo-Gravimetric Analysis(TG), Infrared Spectroscopy(IR) 등이 사용되나, 산업부산물의 특성에 따라 CO2 배출량을 과대 또는 과소 평가할 우려가 있다. 본 연구에서는 CaCO3 시료와 고온에서 산화반응에 의해 중량이 증가하는 시료 각각에 carbonate 형태로 함유된 CO2의 함량을 측정하는 방법으로 LOI, TG, IR 및 DTG(Differential Thermo-Gravimetric Analysis) 방법의 신뢰도와 시험방법별 측정결과를 비교 검토하였다. CaCO3 시료에 대해서는 검토한 모든 시험결과는 충분한 수준의 신뢰도를 나타내었다. 반면, 고온에서 중량이 증가하는 시료의 CO2 함량에 대해서는 LOI와 TG는 시료의 CO2 함량을 제대로 평가하지 못했으며, IR은 예측값에 비해 CO2 함량을 과대평가하는 경향을 나타내었으나, DTG에 의한 평가 결과는 예측값에 근사하였다. 이로부터 수 % 미만 수준의 미량의 CO2를 함유하고, carbonate 광물의 분해 배출 온도에서 CO2 배출에 의한 중량 감소 외에도 중량이 변화하는 시료의 경우 DTG를 이용하여 CO2 함량을 구하는 것이 LOI나 TG, IR을 이용한 평가보다 합리적이라고 판단된다.

4-Chloro-2-((E)-(Isopropylimino)methyl)phenol 코발트(II) 착물에 대한 결정 구조 및 열분해 연구 (Crystal Structure and Thermal Decomposition Studies on Cobalt (II) Complex of 4-Chloro-2-((E)-(Isopropylimino)methyl)phenol)

  • Pu, Xiao-Hua
    • 대한화학회지
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    • 제55권3호
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    • pp.341-345
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    • 2011
  • Schiff base 코발트(II) 착물, bis[4-chloro-2-((E)-(isopropylimino) methyl) phenol]cobalt(II), 을 합성하고 단결정 X-ray 회절 분석을 하였다. 코발트 (ii) 합성물의 현상학적, 속도론적 및 기계적 특성은 TG/DTG법으로 연구하였다. 실험 데이터에 기초하여, 활성화 에너지, 지수 앞자리인자, 활성화 엔트로피와 같은 속도론적 파라미터를 계산하였으며, 가장 가능성 있는 메카니즘 함수로는 $g({\alpha})={\alpha}^2$이 추정되었다. 따라서, 모든 분해 단계에서 속도 조절 단계는 1차원 확산 과정(Parabolic model) 이다.

Implications of SPION and NBT Nanoparticles upon In Vitro and In Situ Biodegradation of LDPE Film

  • Kapri, Anil;Zaidi, M.G.H.;Goel, Reeta
    • Journal of Microbiology and Biotechnology
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    • 제20권6호
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    • pp.1032-1041
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    • 2010
  • The comparative influence of two nanoparticles [viz., superparamagnetic iron oxide nanoparticles (SPION) and nanobarium titanate (NBT)] upon the in vitro and in situ low-density polyethylene (LDPE) biodegradation efficiency of a potential polymer-degrading microbial consortium was studied. Supplementation of 0.01% concentration (w/v) of the nanoparticles in minimal broth significantly increased the bacterial growth, along with early onset of the exponential phase. Under in vitro conditions, ${\lambda}$-max shifts were quicker with nanoparticles and Fourier transform infrared spectroscopy (FTIR) illustrated significant changes in CH/$CH_2$ vibrations, along with introduction of hydroxyl residues in the polymer backbone. Moreover, simultaneous thermogravimetric-differential thermogravimetry-differential thermal analysis (TG-DTG-DTA) reported multiple-step decomposition of LDPE degraded in the presence of nanoparticles. These findings were supported by scanning electron micrographs (SEM), which revealed greater dissolution of the film surface in the presence of nanoparticles. Furthermore, progressive degradation of the film was greatly enhanced when it was incubated under soil conditions for 3 months with the nanoparticles. The study highlights the significance of bacteria-nanoparticle interactions, which can dramatically influence key metabolic processes like biodegradation. The authors also propose the exploration of nanoparticles to influence various other microbial processes for commercial viabilities.

Implications of Fullerene-60 upon in-vitro LDPE Biodegradation

  • Sah, Aditi;Kapri, Anil;Zaidi, M.G.H.;Negi, Harshita;Goel, Reeta
    • Journal of Microbiology and Biotechnology
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    • 제20권5호
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    • pp.908-916
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    • 2010
  • Fullerene-60 nanoparticles were used for studying their effect on the low-density polyethylene (LDPE) biodegradation efficiency of two potential polymer-degrading consortia comprising three bacterial strains each. At a concentration of 0.01% (w/v) in minimal broth lacking dextrose, fullerene did not have any negative influence upon the consortia growth. However, fullerene was found to be detrimental for bacterial growth at higher concentrations (viz., 0.25%, 0.5%, and 1%). Although addition of 0.01% fullerene into the biodegradation assays containing 5mg/ml LDPE subsided growth curves significantly, subsequent analysis of the degraded products revealed an enhanced biodegradation. Fourier transform infrared spectroscopy (FT-IR) revealed breakage and formation of chemical bonds along with the introduction of ${\nu}C$-O frequencies into the hydrocarbon backbone of LDPE. Moreover, simultaneous thermogravimetric-differential thermogravimetry-differential thermal analysis (TG-DTG-DTA) revealed a higher number of decomposition steps along with a 1,000-fold decrease in the heat of reactions (${\Delta}H$) in fullerene-assisted biodegraded LDPE, suggesting the probable formation of multiple macromolecular byproducts. This is the first report whereby fullerene-60, which is otherwise considered toxic, has helped to accelerate the polymer biodegradation process of bacterial consortia.

Bifunctional Fe-SBA-15-SO3H Mesoporous Catalysts with Different Si/Fe Molar Ratios: Synthesis, Characterization and Catalytic Activity

  • Erdem, Sezer;Erdem, Beyhan;Oksuzoglu, Ramis Mustafa;Citak, Alime
    • Bulletin of the Korean Chemical Society
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    • 제34권5호
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    • pp.1481-1486
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    • 2013
  • Bifunctional Fe-SBA-15-$SO_3H$ mesoporous materials with different Si/Fe molar ratios (3, 5, and 7) have been synthesized via a simple direct hydrothermal method and characterized by XRD, $N_2$-adsorption/desorption, TG/DTG and FT-IR techniques, and used as solid acid catalysts in the esterification of lactic acid with methanol. XRD and $N_2$ sorption characterizations show successful iron doping within the mesoporous channels of SBA-15-$SO_3H$. The FT-IR and TG/DTG characterizations also reveal the presence of iron. With the incorporation of Fe ions into the SBA-15-$SO_3H$, the acid sites substantially increased because of the self-separated acidity of the hydrolysis of $Fe^{3+}$ solutions. However, in the Si/Fe = 3 molar ratio, the catalytic conversion decreased which is caused by the reduced cooperation effect between the acid pairs due to the weakened hydrogen bonds and collapse of the pore structure. This further suggests that the mesoporous structure decreases with the decrease in Si/Fe ratio.

Determination of reaction kinetics during vitrification of radioactive liquid waste for different types of base glass

  • Suneel, G.;Rajasekaran, S.;Selvakumar, J.;Kaushik, Chetan P.;Gayen, J.K.;Ravi, K.V.
    • Nuclear Engineering and Technology
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    • 제51권3호
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    • pp.746-754
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    • 2019
  • Vitrification of radioactive liquid waste (RLW) provides a feasible solution for isolating radionuclides from the biosphere for an extended period. In vitrification, base glass and radioactive waste are added simultaneously into the melter. Determination of heat and mass transfer rates is necessary for rational design and sizing of melter. For obtaining an assured product quality, knowledge of reaction kinetics associated with the thermal decomposition of waste constituents is essential. In this study Thermogravimetry (TG) - Differential Thermogravimetry (DTG) of eight kinds of nitrates and two oxides, which are major components of RLW, is investigated in the temperature range of 298-1273 K in the presence of base glasses of five component (5C) and seven component (7C). Studies on thermal behavior of constituents in RLW were carried out at heating rates ranging from 10 to $40\;K\;min^{-1}$ using TG - DTG. Thermal behavior and related kinetic parameters of waste constituents, in the presence of 5C and 7C base glass compositions were also investigated. The activation energy, pre-exponential factor and order of the reaction for the thermal decomposition of 24% waste oxide loaded glasses were estimated using Kissinger method.

Comparison Study of Thermal Decomposition Characteristics of Wattle & Pine Tannin-based Adhesives

  • Kim, Sumin;Lee, Young-kyu;Kim, Hyun-Joong;Eom, Young Geun
    • Journal of the Korean Wood Science and Technology
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    • 제30권3호
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    • pp.34-41
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    • 2002
  • This study investigated the thermogravimetric analysis of two types of cured tannin-based adhesives from wattle and pine, with three hardeners of paraformaldehyde, hexamethylenetetramine and TN (tris(hydroxyl)nitromethan), at a temperature of 170℃ and a heating rate of 5, 10, 20 and 40℃/min for 10 minutes. The 5 minutes cured wattle tannin-based adhesive with each hardener at 170℃ was also tested to compare the degree of curing. It was found that thermogravimetric analysis could be used to measure the degree of curing of a thermosetting adhesive. The TG-DTG curves of all the adhesive systems were similar and showed three steps in a similar way to a phenolic resin. This means that each adhesive system is well cross-linked. However, a high thermal decomposition rate was shown at 150 to 400℃ in the case of the pine tannin sample with TN (tris(hydroxyl)nitromethan). The Flynn & Wall expression was used to evaluate the activation energy for thermal decomposition. As the level of conversion (𝛼) increased, the activation energy of each system increased. The activation energy of the wattle tannin-based adhesive with paraformaldehyde was higher than the others.

국산 침·활엽수재의 열분해 및 해부학적 특성에 관한 연구 (A Study on Pyrolytic and Anatomical Characteristics of Korean Softwood and Hardwood)

  • 김대영;강성호;정헌영
    • Journal of the Korean Wood Science and Technology
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    • 제35권6호
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    • pp.31-42
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    • 2007
  • 국산 침 활엽수재의 열분해 및 해부학적 특성에 관해 조사하기 위해 침엽수재 3종(소나무, 리기다소나무, 낙엽송) 및 활엽수재 3종(단풍나무, 물푸레나무, 굴참나무)의 화학적 성분분석, TG-DTA (Thermogravimetric Analysis & Differential Thermal Analysis), 메틸렌블루 흡착성능(MBA) 및 SEM 관찰을 하였다. TG-DTA에서 시료는 $1{\ell}/min$$N_2$ 가스가 유입되는 조건하에 $10^{\circ}C$/min의 숭온속도로 최대 $10^{\circ}C$까지 탄화되었다. 화학적 성분분석 결과 모든 시료에서 전형적인 목재 주성분의 함량을 나타냈다. TG-DTA 결과, 침엽수재의 탄화수율이 활엽수보다 높았으며 목재 주성분 중 리그닌의 탄화수율이 가장 높았다. 모든 시료가 전형적인 목재 열분해의 TGA, DTG, DTA 곡선을 나타냈지만, 침 활엽수재 간에 몇 가지 차이점이 나타났다. 리그닌의 함량이 열분해에 큰 영향을 미쳤으며, 리그닌의 분자구조에 따라 중량감소와 탄화수율이 크게 달라졌다. 메틸렌블루 흡착성능 시험 결과 침엽수재의 MBA가 활엽수재보다 높았으며 소나무의 MBA가 가장 높았지만, 활성탄이나 백탄보다는 약 23배, 4씩 낮았다. SEM 관찰 결과 탄화 과정에서 전체적인 목재의 구조와 목재 섬유의 섬유구조가 그대로 유지됨을 확인하였다.

Kinetic Analysis for the Catalytic Pyrolysis of Polyethylene Terephthalate Over Cost Effective Natural Catalysts

  • Pyo, Sumin;Hakimian, Hanie;Kim, Young-Min;Yoo, Kyung-Seun;Park, Young-Kwon
    • 공업화학
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    • 제32권6호
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    • pp.706-710
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    • 2021
  • In the current research, thermal and catalytic thermogravimetric (TG) analysis of polyethylene terephthalate (PET) over natural zeolite (NZ), olivine, bentonite, HZSM-5, and HAl-MCM-41 were investigated using a TG analyzer and model-free kinetic analysis. Catalytic TG analysis of PET was carried out at multi-heating rates, 10, 20, 30, and 40 ℃/min, under nitrogen atmosphere. Apparent activation energy (Ea) values for the thermal and catalytic pyrolysis of PET were calculated using Flynn-Wall-Ozawa method. Although natural catalysts, NZ, olivine, and bentonite, could not lead the higher PET decomposition efficiency than synthetic zeolites, HZSM-5 and HAl-MCM-41, maximum decomposition temperatures on the differential TG (DTG) curves for the catalytic pyrolysis of PET, 436 ℃ over olivine, 435 ℃ over bentonite, and 434 ℃ over NZ, at 10 ℃/min, were definitely lower than non-catalytic pyrolysis. Calculated Ea values for the catalytic pyrolysis of PET over natural catalysts, 177 kJ/mol over olivine, 168 kJ/mol over bentonite, and 171 kJ/mol over NZ, were also not lower than those over synthetic zeolites, however, those were also much lower than the thermal decomposition, suggesting their feasibility as the proper and cost-effective catalysts on the pyrolysis of PET.