• 자연과학논문집
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• 제1권
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• pp.47-59
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• 1987

티타닐 옥살산 바륨 사 수화물(BaTiO($$C_2$$O_4$)_2$ $4H_2$O) 의 분해반응을 열중량 분석법 (TG), 미분 열중량 분석법 (DTG) 그리고 시차 열분석법 (DTA) 를 이용하여 반응기구를 조사 하였다. 중간 생성물과 생성기체는 적외선 분광법과 X-ray회절법을 이용하여 확인하였다. 열분해 과정은 탈수 과정을 포함하여 5단계 분해과정으로 진행하였으며 1단계 분해과정은 탈수과정이며 일부 옥살산기의 분해과정이 함께 일어나게 된다. 2단계 분해과정에서는 1/2몰의 일산화 탄소가 방출되었다. 옥살산기의 분해는 $260~460^{\circ}C$의 온도범위에서 완전히 일어나고 분해하는 시료의 중간체에 자유로운 이산화 탄소기를 가지는 탄산화물을 생성하게 된다. 중간 생성체인 탄산화물의 최종분해는 $650~750^{\circ}C$에서 일어나며 티탄산 바륨 ($BaTiO_3$)이 생성된다.

• 대한화학회지
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• 제57권1호
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• pp.52-62
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• 2013

The interaction of titanium (IV), yttrium (III), zirconium (IV), palladium (II) and cerium (IV) with deprotonated enrofloxacin leads to the formation of the neutral or cationic mononuclear complexes. The isolated solid complexes have been characterized with physicochemical and spectroscopic techniques and thermogravimeteric analyses. The spectroscopic data indicate that the enrofloxacin ligand is on the deprotonated mode acting as bidentate ligand coordinated to the metal ions through the ketone oxygen and a carboxylato oxygen and the metal ions completed the coordination number with water molecules. The thermal decomposition mechanisms proposed for enrofloxacin and their metal complexes were discussed. The activation energies, $E^*$, enthalpies, ${\Delta}H^*$, entropies, ${\Delta}S^*$ and Gibbs free energies, ${\Delta}G^*$, of the thermal decomposition reactions have been derived from thermogravimetric (TG) and differential thermogravimetric (DTG) curves, using Coats-Redfern (CR) and Horowitz-Metzeger (HM) methods. The antimicrobial activity has been evaluated against six different microorganisms.

• Bulletin of the Korean Chemical Society
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• 제25권1호
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• pp.45-50
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• 2004

$Cu^{II}$-complexes of N-salicylideneaniline and its derivatives were not light sensitive in most solvents such as acetonitrile. A photo-decomposition occurred upon irradiation in halocarbon solvents such as $CHCl_3$. It has been suggested that such photoreactivity is attributed to the reactivity of charge-transfer to solvent (CTTS) excited state attained upon irradiation. A mechanism has been proposed to account for the results obtained. The complexes have been thermally analysed in nitrogen and static air using thermogravimetry (TG) and derivative thermogravimetry (DTG). The thermal degradation of the complexes proceeds in two or three stages. The kinetic parameters obtained from the Coats-Redfern and Horowitz-Metzger equations show the kinetic compensation effect.

• Bulletin of the Korean Chemical Society
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• 제32권9호
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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.

• 대한화학회지
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• 제38권2호
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• pp.92-100
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• 1994

초미립 코발트 치환 산화철 분말을 새로운 유기금속 전구체인 $Co_xFe_{1-x}(N_2H_3COO)_2(N_2H_4)_2$ (x = 0, 0.01, 0.02, 0.03, 0.05, 0.10, 1.00)을 열분해화 산화과정으로 제조하였다.유기금속 전구체는 몰비 x : 1-x인 Co(II)와 Fe(II)를 hydrazinocarboxylic acid와 반응시켜서 합성하였고, 합성을 정량분석, 및 적외선분광기를 사용하며, 합성을 정량분석, 원소분석 및 적외선분광기를 사용하여 확인하였다. 유기금속 전구체의 열분해 과정은 TG-DTG 와 DSC로 살펴보았다. 코발트치환 산화철 분말은 유기금속 전구체를 대기 중에서 $350^{\circ}C$ 와 $450^{\circ}C$에서 6시간 열처리하여 제조하였다. 산화철의 결정상은 각각 ${\gamma}-Fe_2O_3$ 및 ${\gamma}-Fe_2O_3$ 와 ${\alpha}-Fe_2O_3$의 혼합상이었다. 입자의 형태는 구형에 가까운 모양이었고 크기는 $0.05{\mu}m$ 이하의 초미립이었다. 코발트 치환 산화철의 보자력과 각형비는 코발트 함량 또는 열처리 온도가 높아질 수록 증가하였다.

• 대한화학회지
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• 제55권4호
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• pp.612-619
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• 2011

1,2-diphenyl-4-butyl-3,5-pyrazolidinedione(phenylbutazone, PB)의 란탄(III) 착물을 합성하여 원소분석, 몰전기전도도 측정, IR, UV-Vis. 및 NMR 스펙트럼으로 특성을 조사하였다. 스펙트럼 데이터로부터 PB가 pyrazolidinedione 고리의 두 카르보닐 산소를 통해 이배위 및 일이온화 리간드로 배위됨을 규명하였다. 몰전기전도도 데이터로부터 이들 착물이 비전해질임을 규명하였다. 이들 착물의 열적 행동을 공기 중에서 TG 및 DTG로 연구한 결과, 탈수화, 열적 안전성 및 열분해에 관한 정보를 얻을 수 있었다. 최종 생성물은 해당 금속의 산화물로 밝혀졌다. 탈수화 및 분해 단계에 대한 열역학 및 반응속도 파라메터를 구하였다. 분해 단계에 대한 음의 엔트로피 값은 반응물보다 활성화 착물이 더 질서있는 구조를 갖는다는 것을 의미하며, 이때 반응은 정상보다 느렸다. 이러한 연구를 바탕으로 착물의 분자식이 $[Ln(PB)_3]{\cdot}5H_2O$(Ln=La 및 Ce) 그리고 $[Ln(PB)_3 (H_2O)_2]{\cdot}2H_2O$(Ln=Pr, Nd 및 Sm)임을 규명하였다.

• 한국산학기술학회논문지
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• 제20권2호
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• pp.451-457
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• 2019

본 연구는 커피박을 열풍건조와 유중건조 방법을 통해 고형연료로 제조하여 특성고찰을 진행하였다. 그리고 각 건조시료의 발열량 차이를 비교였다. 그리고 열중량분석기를 이용한 공업분석법이 유기성 폐기물 및 유중처리 시료에 적용 여부를 고찰하였다. 그 결과, 로 내부를 $N_2$ 분위기에서 $100^{\circ}C$까지 가열한 후 180분 동안 유지한다. 그 후 $100^{\circ}C$에서 $950^{\circ}C$까지 가열하고 $950^{\circ}C$에서 7분 동안 유지한다. 이후 $600^{\circ}C$로 냉각하고 로 내부를 $O_2$ 분위기로 전환한다. 그리고 $815^{\circ}C$에서 30분 내 외로 온도를 유지하는 것이 적당하다. 다음으로 건조 전과 후 시료의 표면을 SEM장비로 관찰하였고 EDS 장비를 통해 성분을 측정하였다. 그 결과 중금속과 같은 기타 유해성분은 측정되지 않았다. 그리고 열중량분석기를 통해 TG와 DTG 곡선을 얻었고 이를 통해 열분해와 연소반응의 차이점을 고찰하였다. 그 결과, 유중건조 된 커피박이 열풍건조 된 커피박 보다 착화 시간이 긴 것으로 보인다. 마지막으로, 열중량분석기에서 배출되는 연소가스를 포집하여 시간에 따른 CO와 $CO_2$ 농도를 GC를 이용하여 정성 및 정량분석 하였다.

• Current Research on Agriculture and Life Sciences
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• 제31권1호
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• pp.18-24
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• 2013

This work attempted to fabricate organic/inorganic nanocomposite by combining organic cellulose nanofibrils (CNFs), isolated by 2,2,6,6-tetramethylpiperidine-1-oxy radical (TEMPO)-mediated oxidation of native cellulose with inorganic nanoclay. The morphology and dimension of CNFs, and tensile properties and thermal stability of CNF/clay nanocomposites were characterized by transmission electron microscope (TEM), tensile test, and thermogravimetry (TG), respectively. TEM observation showed that CNFs were fibrillated structure with a diameter of about $4.86{\pm}1.341nm$. Tensile strength and modulus of the hybrid nanocomposite decreased as the clay content of the nanocomposite increased, indicating a poor dispersion of CNFs or inefficient stress transfer between the CNFs and clay. The elongation at break increased at 1% clay level and then continuously decreased as the clay content increased, suggesting increased brittleness. Analysis of TG and derivative thermogravimetry (DTG) curves of the nanocomposites identified two thermal degradation peak temperatures ($T_{p1}$ and $T_{p2}$), which suggested thermal decomposition of the nanocomposites to be a two steps-process. We think that $T_{p1}$ values from $219.6^{\circ}C$ to $235^{\circ}C$ resulted from the sodium carboxylate groups in the CNFs, and that $T_{p2}$ values from $267^{\circ}C$ to $273.5^{\circ}C$ were mainly responsible for the thermal decomposition of crystalline cellulose in the nanocomposite. An increase in the clay level of the CNF/clay nanocomposite predominately affected $T_{p2}$ values, which continuously increased as the clay content increased. These results indicate that the addition of clay improved thermal stability of the CNF/clay nanocomposite but at the expense of nanocomposite's tensile properties.

• Bulletin of the Korean Chemical Society
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• 제33권8호
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• pp.2724-2730
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• 2012

A new heterogeneous acidic catalyst was successfully prepared by impregnation of silica (Aerosil 300) by an acidic ionic liquid, named 1-(4-sulfonic acid)butylpyridinium hydrogen sulfate [$PYC_4SO_3H$][$HSO_4$], and characterized using FT-IR spectroscopy, the $N_2$ adsorption/desorption analysis (BET), thermal analysis (TG/DTG), and X-ray diffraction (XRD) techniques. The amount of loaded acidic ionic liquid on Aerosil 300 support was determined by acid-base titration. This new solid acidic supported heterogeneous catalyst exhibits excellent activity in the synthesis of 2-aryl-2,3-dihydroquinazolin-4(1H)-ones by cyclocondensation reaction of 2-aminobenzamide with aromatic aldehydes under solvent-free conditions and the desired products were obtained in very short reaction times with high yields. This catalyst has the advantages of an easy catalyst separation from the reaction medium and lower problems of corrosion. Recycling of the catalyst and avoidance of using harmful organic solvent are other advantages of this simple procedure.

• 대한화학회지
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• 제58권2호
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• pp.169-178
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• 2014

A new series of metal complexes of V(IV), Pd(II), Pt(IV), Ce(IV) and U(VI) with 3-[(3-chlorophenyl)-hydrazono]-pentane-2,4-dione (Cphpd) were synthesized and characterized by elemental analysis, molar conductivity, magnetic moment measurements, UV-vis, FT-IR and $^1H$ NMR as well as TG-DTG techniques. The data indicated that the Cphpd acts as a bidentate ligand through the hydrazono nitrogen and one keto oxygen. The kinetic parameters have been evaluated by using Coats Redfern (CR) and Horowitz-Metzeger (HM) methods. The thermodynamic data reflected the thermal stability for all complexes. The calculated bond length and the bond stretching force constant, F(U=O), values for $UO_2$ bond are $0.775{\AA}$ and $286.95Nm^{-1}$. The bond lengths, bond angles, dipole moment and the lowest energy model structure of the complexes have been determined with DFT calculations. The antimicrobial activity of the synthesized ligand and its complexes were screened.