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Phenylbutazone의 란탄(III) 착물에 대한 합성, 스펙트럼 및 열적 연구
Anoop, M.R.,Binil, P.S.,Jisha, K.R.,Suma, S.,Sudarsanakumar, M.R. 대한화학회 2011 대한화학회지 Vol.55 No.4
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. Lanthanide(III) complexes of 1,2-diphenyl-4-butyl-3,5-pyrazolidinedione(phenylbutazone, PB) have been synthesized and characterized by elemental analyses, molar conductance measurements, IR, UV-Vis. and NMR spectra. The spectral data reveal that the PB acts as a bidentate and mono-ionic ligand coordinating through both the carbonyl oxygens of the pyrazolidinedione ring. The molar conductance data suggest that the complexes are non-electrolytes. The thermal behaviour of the complexes was studied by TG and DTG in air atmosphere and the results provide information about dehydration, thermal stability and thermal decomposition. The final products are found to be the corresponding metal oxides. The thermodynamic parameters and kinetic parameters were evaluated for the dehydration and decomposition stages. The negative entropy values of the decomposition stages indicate that the activated complexes have a more ordered structure than the reactants and that the reactions are slower than normal. Based on these studies, the complexes have been formulated as $[Ln(PB)_3]{\cdot}5H_2O$(Ln=La and Ce) and $[Ln(PB)_3(H_2O)_2]{\cdot}2H_2O$(Ln=Pr, Nd and Sm).
Lithium Insertion Behavior of Nanoscopic Co_3O_4 Prepared with Avian Egg Membrane as a Template
Maria Christy,Jisha. M. R,김애란,남기석,유동진,서은경,T. Sri Devi Kumari,T. Prem Kumar,A. Manuel Stephan 대한화학회 2011 Bulletin of the Korean Chemical Society Vol.32 No.4
Nanoscopic Co_3O_4 particles were prepared using avian egg membrane as a template at 800 °C. The prepared materials were subjected to XRD, SEM, TEM and Raman spectroscopic studies. Cyclic voltammetry study shows a single step oxidation and reduction process. Electrochemical lithium insertion behavior of the materials was examined in coin cells of the 2032 configuration. The material showed a discharge capacity 600mAh/g even after 20 cycles.
Christy, Maria,Jisha, M.R,Kim, Ae-Rhan,Nahm, Kee-Suk,Yoo, Dong-Jin,Suh, E.K.,Kumari, T. Sri Devi,Kumar, T. Prem,Stephan, A. Manuel Korean Chemical Society 2011 Bulletin of the Korean Chemical Society Vol.32 No.4
Nanoscopic $Co_3O_4$ particles were prepared using avian egg membrane as a template at $800^{\circ}C$. The prepared materials were subjected to XRD, SEM, TEM and Raman spectroscopic studies. Cyclic voltammetry study shows a single step oxidation and reduction process. Electrochemical lithium insertion behavior of the materials was examined in coin cells of the 2032 configuration. The material showed a discharge capacity 600mAh/g even after 20 cycles.