• Title/Summary/Keyword: Thermal gravimetric analysis

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Synthesis Gas Production from Gasification of Woody Biomass (목질계 바이오매스로부터 가스화에 의한 합성가스 제조 연구)

  • Cho, Won-Jun;Mo, Yong-Gi;Song, Taek-Yong;Baek, Young-Soon;Kim, Seung-Soo
    • Transactions of the Korean hydrogen and new energy society
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    • v.21 no.6
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    • pp.587-594
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    • 2010
  • Hydrogen is an alternative fuel for the future energy which can reduce pollutants and greenhouse gases. Synthesis gas has played an important role of synthesizing the valuable chemical compounds, for example methanol, DME and GTL chemicals. Renewable biomass feedstocks can be potentially used for fuel and chemicals. Current thermal processing techniques such as fast pyrolysis, slow pyrolysis, and gasification tend to generate products with a large slate of compounds. Lignocellulose feedstocks such as forest residues are promising for the production of bio-oil and synthesis gas. Pyrolysis and gasification was investigated using thermogravimetric analyzer (TGA) and bubbling fluidized bed gasification reactor to utilize forest woody biomass. Most of the materials decomposed between $320^{\circ}C$ and $380^{\circ}C$ at heating rates of $5{\sim}20^{\circ}C$/min in thermogravimetric analysis. Bubbling fluidized bed reactor was used to study gasification characteristics, and the effects of reaction temperature, residence time and feedstocks on gas yields and selectivities were investigated. With increasing temperature from $750^{\circ}C$ to $850^{\circ}C$, the yield of char decreased, whereas the yield of gas increased. The gaseous products consisted of mostly CO, $CO_2$, $H_2$ and a small fraction of $C_1-C_4$ hydrocarbons.

Preparation of Anatase TiO2 Thin Films with (OiPr)2Ti(CH3COCHCONEt2)2 Precursor by MOCVD

  • Bae, Byoung-Jae;Lee, Kwang-Yeol;Seo, Won-Seok;Miah, Md. Arzu;Kim, Keun-Chong;Park, Joon T.
    • Bulletin of the Korean Chemical Society
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    • v.25 no.11
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    • pp.1661-1666
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    • 2004
  • The reaction of titanium tetraisopropoxide with 2 equiv of N,N-diethyl acetoacetamide affords Ti($O^iPr)_2(CH_3COCHCONEt_2)_2$ (1) as colorless crystals in 80% yield. Compound 1 is characterized by spectroscopic (Mass and $^1H/^{13}C$ NMR) and microanalytical data. Molecular structure of 1 has been determined by a single crystal X-ray diffraction study, which reveals that it is a monomeric, cis-diisopropoxide and contains a six coordinate Ti(IV) atom with a cis($CONEt_2$), trans($COCH_3$) configuration (1a) in a distorted octahedral environment. Variable-temperature $^1H$ NMR spectra of 1 indicate that it exists as an equilibrium mixture of cis, trans (1a) and cis, cis (1b) isomers in a 0.57 : 0.43 ratio at -20$^{\circ}C$ in toluene-$d_8$ solution. Thermal properties of 1 as a MOCVD precursor for titanium dioxide films have been evaluated by thermal gravimetric analysis and vapor pressure measurement. Thin films of pure anatase titanium dioxide (after annealing above 500$^{\circ}C$ under oxygen) have been grown on Si(100) with precursor 1 in the substrate temperature range of 350- 500$^{\circ}$ using a bubbler-based MOCVD method.

Influence of fly ash and GGBFS on the pH value of cement mortar in different curing conditions

  • Shafigh, Payam;Yousuf, Sumra;Ibrahim, Zainah;Alsubari, Belal;Asadi, Iman
    • Advances in concrete construction
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    • v.11 no.5
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    • pp.419-428
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    • 2021
  • The pH of cement-based materials (CBMs) is an important factor for their durability, sustainability, and long service life. Currently, the use of supplementary cementitious materials (SCMs) is becoming mandatory due to economic, environmental, and sustainable issues. There is a decreasing trend in pH of CBMs due to incorporation of SCMs. The determination of numerical values of pH is very important for various low and high volume SCMs blended cement mortars for the better understanding of different defects and durability issues during their service life. In addition, the effect of cement hydration and pozzolanic reaction of SCMs on the pH should be determined at initial and later ages. In this study, the effect of low and high-volume fly ash (FA) and ground granulated ballast furnace slag (GGBFS) cement mortars in different curing conditions on their pH values has been determined. Thermal gravimetric analysis (TGA) was carried out to support the findings from pH measurements. In addition, thermal conductivity (k-value) and strength activity indices of these cement mortars were discussed. The results showed that pH values of all blended cement mortars were less than ordinary Portland cement (OPC) mortar in all curing conditions used. There was a decreasing tendency in pH of all mortars with passage of time. In addition, the pH of cement mortars was not only dependent on the quantity of Ca(OH)2. The effect of adding SCMs on the pH value of cement mortar should be monitored and measured for both short and long terms.

Thermal behavior of $PrCl_3$ in an oxidizing condition (산화조건에서 $PrCl_3$의 열적거동)

  • Eun, Hee-Chul;Yang, Hee-Chul;Cho, Yong-Zun;Lee, Han-Soo;Kim, In-Tae
    • Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
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    • v.7 no.4
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    • pp.207-212
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    • 2009
  • In this study, a thermal behavior of $PrCl_3$ as one of the lanthanide chlorides in LiCl-KCl molten salts was investigated in an oxidizing condition. First, a thermo-gravimetric analysis (TGA) of $PrCl_3$ was carried out by an injection of $O_2$ gas. Based on the results, an oxidation of $PrCl_3$ in the molten salts was performed by sparging $O_2$ gas with changing temperatures. According to the TGA data of $PrCl_3$, a dissociation of $PrCl_3$ occurred rapidly by about $380^{\circ}C$ and a conversion of $PrCl_3$ to $PrCl_3$ was completed at about $600^{\circ}C$. The thermal behavior of $PrCl_3$ in LiCl-KCl molten salts by sparging $O_2$ gas was similar to that of $PrCl_3$ in the TGA test, and PrOCl as a insoluble compound in the molten salts was precipitated into the bottom of the molten salts. A conversion of $PrCl_3$ to PrOCl in the molten salts occurred actively at a higher temperature than $650^{\circ}C$. And it would be possible to estimate a conversion status of $PrCl_3$ to PrOCl by measuring a $Cl_2$ concentration in a flue gas generated from an oxidation test of $PrCl_3$ in LiCl-KCl molten salts.

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Effects of NaCl/H3PO4 Flame Retardant Treatment on Lyocell Fiber for Thermal Stability and Anti-oxidation Properties (NaCl/H3PO4 내염화 처리가 라이오셀 섬유의 열 안정 및 내산화 특성에 미치는 영향)

  • Kim, Eun Ae;Bai, Byong Chol;Jeon, Young-Pyo;Lee, Chul Wee;Lee, Young-Seak;In, Se Jin;Im, Ji Sun
    • Applied Chemistry for Engineering
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    • v.25 no.4
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    • pp.418-424
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    • 2014
  • The improved thermal stability and anti-oxidation properties of Lyocell fiber were studied based on flame retardant treatment by using NaCl/$H_3PO_4$ solution. The optimized conditions of flame retardant treatment were studied on various maxing ratio of NaCl and $H_3PO_4$ and the mechanism was proposed through experimental results of thermal stability anti-oxidation. The IPDT (integral procedural decomposition temperature), LOI (limited oxygen index) and $E_a$ (activation energy) increased 23, 30 and 24% respectively via flame retardant treatment. It is noted that thermal stability and anti-oxidation improved based on char and carbon layer formation by dehydrogenation and dissociation of C-C bond resulting the hindrance of oxygen and heat energy into polymer resin. The optimized conditions for efficient flame retardant property of Lyocell fiber were provided using NaCl/$H_3PO_4$ solution and the mechanism was also studied based on experimental results such as IDT (initial decomposition temperature), IPDT, LOI and $E_a$.

Na3PO4 Flame Retardant Treatment on Lyocell Fiber for Thermal Stability and Anti-oxidation Properties (라이오셀의 열 안정 및 내산화 특성 향상을 위한 Na3PO4 내염화 처리)

  • Kim, Hyeong Gi;Kim, Eun Ae;Lee, Young-Seak;In, Se Jin
    • Fire Science and Engineering
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    • v.29 no.2
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    • pp.25-32
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    • 2015
  • The improved thermal stability and anti-oxidation properties of lyocell fiber were studied based on flame retardant treatment by using $Na_3PO_4$ solution. The optimized conditions of flame retardant treatment were studied on various concentrations of $Na_3PO_4$ and the mechanism was proposed through experimental results of thermal stability and anti-oxidation. The integral procedural decomposition temperature (IPDT), limiting oxygen index (LOI) and activation energy ($E_a$) increased 30, 160% respectively via flame retardant treatment. It is noted that thermal stability and anti-oxidation improved based on char and carbon layer formation by dehydrogenation and dissociation of C-C bond resulting the hindrance of oxygen and heat energy into polymer resin. The optimized conditions for efficient flame retardant property of lyocell fiber were provided using $Na_3PO_4$ solution and the mechanism was also studied based on experimental results such as initial decomposition temperature (IDT), IPDT, LOI and $E_a$.

A Study about the Strength and Microstructure of Hardened Cement Pastes Including Nanofibers (나노 섬유를 혼합한 시멘트 페이스트의 미세구조와 강도에 대한 연구)

  • Nguyen, Tri N.M;Kim, Jung Joong
    • KSCE Journal of Civil and Environmental Engineering Research
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    • v.40 no.2
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    • pp.177-182
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    • 2020
  • In this study, the effect of nanofibers in cement pastes on the compressive and tensile strength of hardened cement pastes was studied. Two types of nanofibers, nylon 66 nanofibers and carbon nanotube-nylon 66 hybrid nanofibers, were manufactured by electrospinning methodology and mixed in cement powder respectively. The specimens for experiments were prepared by water to cement ratio of 0.5 and cured in water for 28 days. The effect of nanofibers on the increase of the compressive and tensile strength were confirmed by the experimental results. The well-linking effect of nanofibers in the microstructure of the hardened cement pastes has been found by scanning electron microscope (SEM) analysis and well-explained for the increase in mechanical strength. Besides, field emission transmission electron microscope (FE-TEM) analysis and thermal gravimetric analysis (TGA) have also been conducted to analyze the properties of nanofibers as well as the microstructure of the hardened modified cement pastes.

A STUDY ON OXIDATION TREATMENT OF URANIUM METAL CHIP UNDER CONTROLLING ATMOSPHERE FOR SAFE STORAGE

  • Kim, Chang-Kyu;Ji, Chul-Goo;Bae, Sang-Oh;Woo, Yoon-Myeoung;Kim, Jong-Goo;Ha, Yeong-Keong
    • Nuclear Engineering and Technology
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    • v.43 no.4
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    • pp.391-398
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    • 2011
  • The U metal chips generated in developing nuclear fuel and a gamma radioisotope shield have been stored under immersion of water in KAERI. When the water of the storing vessels vaporizes or drains due to unexpected leaking, the U metal chips are able to open to air. A new oxidation treatment process was raised for a long time safe storage with concepts of drying under vacuum, evaporating the containing water and organic material with elevating temperature, and oxidizing the uranium metal chips at an appropriate high temperature under conditions of controlling the feeding rate of oxygen gas. In order to optimize the oxidation process the uranium metal chips were completely dried at higher temperature than $300^{\circ}C$ and tested for oxidation at various temperatures, which are $300^{\circ}C$, $400^{\circ}C$, and $500^{\circ}C$. When the oxidation temperature was $400^{\circ}C$, the oxidized sample for 7 hours showed a temperature rise of $60^{\circ}C$ in the self-ignition test. But the oxidized sample for 14 hours revealed a slight temperature rise of $7^{\circ}C$ representing a stable behavior in the self-ignition test. When the temperature was $500^{\circ}C$, the shorter oxidation for 7 hours appeared to be enough because the self-ignition test represented no temperature rise. By using several chemical analyses such as carbon content determination, X-ray deflection (XRD), Infrared spectra (IR) and Thermal gravimetric analysis (TGA) on the oxidation treated samples, the results of self-ignition test of new oxidation treatment process for U metal chip were interpreted and supported.

Variation in optical, dielectric and sintering behavior of nanocrystalline NdBa2NbO6

  • Mathai, Kumpamthanath Chacko;Vidya, Sukumariamma;Solomon, Sam;Thomas, Jijimon Kumpukattu
    • Advances in materials Research
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    • v.2 no.2
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    • pp.77-91
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    • 2013
  • High quality nanoparticles of neodymium barium niobium ($NdBa_2NbO_6$) perovskites have been synthesized using an auto ignition combustion technique for the first time. The nanoparticles thus obtained have been characterized by powder X-ray diffraction, thermo gravimetric analysis, differential thermal analysis, Fourier transform infrared spectroscopy, Raman spectroscopy and transmission electron microscopy. UV-Visible absorption and photoluminescence spectra of the samples are also recorded. The structural analysis shows that the nano powder is phase pure with the average particle size of 35 nm. The band gap determined for $NdBa_2NbO_6$ is 3.9 eV which corresponds to UV-radiation for optical inter band transition with a wavelength of 370nm. The nanopowder could be sintered to 96% of the theoretical density at $1325^{\circ}C$ for 2h. The ultrafine cuboidal nature of nanopowders with fewer degree of agglomeration improved the sinterability for compactness at relatively lower temperature and time. During the sintering process the wide band gap semiconducting behavior diminishes and the material turns to a high permittivity dielectric. The microstructure of the sintered surface was examined using scanning electron microscopy. The striking value of dielectric constant ${\varepsilon}_r=43$, loss factor tan ${\delta}=1.97{\times}10^{-4}$ and the observed band gap value make it suitable for many dielectric devices.

Mass Balance Method for Purity Assessment of Organic Reference Materials: for Thermolabile Materials with LC-UV Method

  • Lee, Joonhee;Kim, Byungjoo
    • Bulletin of the Korean Chemical Society
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    • v.35 no.11
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    • pp.3275-3279
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    • 2014
  • A mass balance method for purity assessment of thermolabile organic reference materials was established by combining several techniques, including liquid chromatography with UV/VIS detector (LC-UV), Karl-Fischer (K-F) Coulometry, and thermal gravimetric analysis (TGA). This method was applied to three fluoroquinolones like enrofloxacin, norfloxacin and ciprofloxacin. LC-UV was used to analyze structurally related organic impurities based on UV/VIS absorbance spectra obtained in combination with LC separation. For all three organic reference materials, the UV/VIS spectra of the separated impurities were similar to that of the major component of the corresponding materials. This indicates that the impurities are structurally related to the respective reference material sharing common chromophores. Impurities could be quantified by comparing their absorbances at the wavelength of maximum absorbance (${\lambda}_{max}$). The water contents of the reference materials were measured by K-F Coulometry by an oven-drying method. The total inorganic impurities contents were assayed from ash residues in TGA analysis with using air as a reagent gas. The final purities estimated from results of those analytical techniques were assigned as ($99.91{\pm}0.06$), ($97.09{\pm}0.17$) and ($91.85{\pm}0.17$)% (kg/kg) for enrofloxacin, norfloxacin and ciprofloxacin, respectively. The assigned final purities would be applied to the reference materials which will be used as calibrators for the certification of those compounds in matrix CRMs as starting points for the traceability of their certified values to SI units.