Síntese, caracterização e estudo do comportamento térmico dos 4-metoxibenzoatos de lantanídeos(III) e ítrio(III), no estado sólido

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Síntese, caracterização e estudo termoanalítico dos 2-metoxibenzalpiruvatos de lantanídios (III), exceto promécio, e de ítrio (III) do estado sólido

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Thermal behaviour of nicotinic acid, sodium nicotinate and its compounds with some bivalent transition metal ions

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Solid-state compounds of 2-methoxybenzylidenepyruvate with some bivalent metal ions - Synthesis, characterization and thermal behavior studies

Solid-state M-2-MeO-BP compounds, where M represents bivalent Mn, Fe, Co, Ni, Cu, Zn and 2-MeO-BP is 2-methoxybenzylidenepyruvate have been synthesized. Simultaneous thermogravinietry-differential thermal analysis (TG-DTA), differential scanning calorimetry (DSC), X-ray powder diffractometry, infrared spectroscopy, elemental analysis and complexometry were used to characterize and to study the thermal stability and thermal decomposition of these compounds. The results led to information about the composition, dehydration, crystallinity and thermal decomposition of the isolated compounds.

Modificação de superfície da liga Ti6A14V para apliacação biomédica

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Síntese, aplicação e avaliação da toxicidade aguda de complexo orgânico à base de európio proposto como marcador fotoluminescente para a Identificação de resíduos de tiro

Um complexo de alta fotoluminescência é proposto como marcador óptico para a identificação de resíduos de tiro (GSR). O marcador é o complexo [Eu(PIC)3(NMK)3], de fórmula molecular Eu(C6H2N3O7)3.(C7H13NO)3, que apresenta o íon Eu3+ e os ligantes ácido pícrico (PIC) e n-metil-Ɛ-caprolactama (NMK). Foi realizada a caracterização quimicamente através de espectroscopia de emissão, espectroscopia de infravermelho com transformada de Fourier (FTIR), termogravimetria e análise térmica diferencial (TG/DTA), e espectrometria de massas com ionização por eletrospray e ressonância ciclotrônica de íons por transformada de Fourier (ESI-FT-ICR MS), e, em seguida, foram adicionadas diferentes massas do complexo a munições convencionais (de 2 a 50 mg por cartucho). Após os tiros, o GSR marcado foi visualmente e quimicamente detectado por irradiação UV (ʎ = 395 nm) e ESI-FT-ICR MS, respectivamente. Os resultados mostraram uma fotoluminescência eficiente e duradoura, sendo facilmente visível sobre a superfície do alvo, no ambiente, no cartucho deflagrado, na arma de fogo, e sobre as mãos e braços do atirador quando utilizada massa a partir de 25 mg do marcador em cartuchos .38 e 50 mg em cartuchos .40. Sua toxicidade aguda também foi avaliada empregando-se o Protocolo 423 da Organização para a Cooperação e Desenvolvimento Econômico (OECD) e apresentou DL50 de 1000 mg.kg-1, sendo classificado como de categoria 4 na escala do Sistema Globalmente Harmonizado de Classificação e Rotulagem de Produtos Químicos (GHS), considerado, portanto, de média toxicidade. O composto mostrou ser menos tóxico do que os componentes inorgânicos de munições convencionais (em especial o Pb), justificando o seu emprego como marcador de GSR.

Estudo da regeneração de aditivos para catalisadores de craqueamento aluminofosfatos (ALPO s)e silicoaluminofosfatos (SAPO s)

Heterogeneous catalysts such as aluminophosphate and silicoaluminophosphate, molecular sieves with AEL of ALPO-11 and SAPO-11, were synthesized by the hydrothermal method with the following molar composition: 2.9 Al +3.2 P + 3.5 DIPA +32.5 H20 (ALPO-11); 2.9 Al +3.2 P + 0.5 Si + 3.5 DIPA +32.5 H20 (SAPO-11) starting from silica (only in the SAPO-11), pseudoboehmite, orthophosphoric acid (85%) and water, in the presence of a di-isopropylamine organic template. The crystallization process occurred when the reactive hydrogel was charged into a vessel and autoclaved at 170ºC for a period of 48 hours under autogeneous pressure. The obtained materials were washed, dried and calcined to remove the molecular sieves of DIPA. The samples were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), infrared spectroscopy (FT-IR), thermo gravimetric differential thermal analysis (TG/DTA) and nitrogen adsorption (BET). The acidic properties were determined using adsorption of n-butylamine followed by programmed thermodessorption. This method revealed that ALPO-11 has weaker acid sites due to structural defects, while SAPO-11 shows an acidity that ranges from weak to moderate. However, a small quantity of strong acid sites could be detected there. The deactivation of the catalysts was conducted by the cracking of the n-hexane in a fixed bed continuous flow microrreator coupled on line to a gas chromatograph. The main products obtained were: ethane, propane, isobutene, n-butane, n-pentane and isopentane. The Vyazovkin (model-free) kinetics method was used to determine the regeneration and removal of the organic template

Deposition and photo-induced electrical resistivity of dip-coated NiO thin films from a precipitation process

Thin films of the semiconductor NiO are deposited using a straightforward combination of simple and versatile techniques: the co-precipitation in aqueous media along with the dip- coating process. The obtained material is characterized by gravimetric/differential thermal analysis (TG-DTA) and X-ray diffraction technique. TG curve shows 30 % of total mass loss, whereas DTA indicates the formation of the NiO phase about 578 K (305 C). X-ray diffraction (XRD) data confirms the FCC crystalline phase of NiO, whose crystallinity increases with thermal annealing temperature. UV-Vis optical absorption measurements are carried out for films deposited on quartz substrate in order to avoid the masking of bandgap evaluation by substrate spectra overlapping. The evaluated bandgap is about 3.0 eV. Current-voltage (I-V) curves measured for different temperatures as well as the temperature-dependent resistivity data show typical semiconductor behavior with the resistivity increasing with the decreasing of temperature. The Arrhenius plot reveals a level 233 meV above the conduction band top, which was attributed to Ni2+ vacancy level, responsible for the p-type electrical nature of NiO, even in undoped samples. Light irradiation on the films leads to a remarkable behavior, because above bandgap light induced a resistivity increase, despite the electron-hole generation. This performance was associated with excitation of the Ni 2+ vacancy level, due to the proximity between energy levels. © 2012 Springer Science+Business Media New York.

Sn(1-x)LaxO2 thin films deposited on AISI 304 stainless steel substrates

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Síntese, caracterização e estudo termoanalítico dos nicotinatos de alguns metais de transição bivalentes no estado sólido

Pós-graduação em Química - IQ

Síntese, caracterização térmica e grau de conversão de polímeros dimetacrilatos com diferentes coiniciadores não tóxicos

The photopolimerization it is be widely used nowadays in different fields as materials, medicine and dentistry. To occur that synthesis is utilized dimethacrylates monomers and photoinitiators, the photoinitiator system more usual is camphorquinone/tertiary amine (ethyl-p-dimethylamino benzoate). However is knowledge that tertiary amines are toxics, so the aim of this work is replace toxic amine compounds to non-toxic compounds as glycerol and inositol. Therefore was used the FTIR technic to calculate the monomers conversion degree as well as Thermogravimetric Analysis-simultaneous differential thermal analysis (TG-DTA) and Differential Scanning Calorimetry (DSC) to evaluate thermal stability, combustion rate, degradation steps, oxidation and volatilization of all samples. The study shown no significant difference about thermal behavior of all polymers, the initiators system for efficient and more fastness was camphorquinone /tertiary amine system followed by ca mph o r quinone/glycerol system

Preparation, characterization and thermal behavior of double selenates of calcium, beryllium and ammonium.

The preparation and thermal decomposition ammonium selenate and calcium and beryllium selenates have been reported previously. However, there are not any information in the literature concerning the thermal decomposition of double selenates of calcium, of beryllium and ammonium. Thermogravimetry (TG), Differential Thermal Analysis (DTA) were used in the studies and characterisation of these compounds.

Synthesis and thermal study of 8-hydroxy-quinoline derivatives of the alkaline Earth metals: I. Strontium complexes

Strontium complexes of 5,7-dibromo-, 5,7-dichloro-, 7-iodo- and 5-chloro-7-iodo-8-hydroxyquinoline were precipitated from an aqueous ammonia and acetone medium. The complexes obtained were Sr[(C9H4ONBr2)2]·2.5H 2O; Sr[(C9H4ONCl2)(OH)]·1.5H2O; Sr[(C9H5ONI)2]·5H2O and Sr[(C9H4ONICl)(OH)]·1.25H2O. The residues of their thermal decomposition were SrBr2; a mixture of SrCl2, SrCO3 and SrO3 SrCO3, and SrCO3, respectively. All were characterized by means of thermogravimetry, differential thermal analysis, complexometry with EDTA, atomic absorption spectroscopy, IR spectroscopy and X-ray diffraction. © 1999 Akadémiai Kiadó.

Thermal decomposition of the hydrated basic carbonates of lanthanides and yttrium

Thermogravimetry, differential thermal analysis, differential scanning calorimetry, IR absorption spectroscopy, X-ray diffraction, and other methods of analysis have been used in the characterization and study of the thermal decomposition of the basic carbonate hydrates of lanthanides and yttrium. These compounds were obtained by precipitation from homogeneous solutions via the hydrolysis of urea, without the addition of an auxiliary anion. The results show that the TG and DTA curves are characteristic for each compound. The results also permit suggestions concerning the compositions and mechanisms of thermal decomposition of these compounds. © 1989.

Thermal analysis of coordination compounds. Part 3. Thermal decomposition of platinum complexes containing triphenylphosphine, triphenylarsine and triphenylstibine

Studies by thermogravimetric analysis (TG) and differential thermal analysis (DTA) of the complexes [PtCl2L2] (L is PPh3, AsPh3, SbPh3), [PtLn] (n = 3, L is SbPh3; n = 4, L is PPh3, AsPh3); [(PtL3)2N2]; [(PtL3)2C2] and [Pt(CO)2L2] (L is SbPh3) are described. Analysis of the TG and DTA curves showed that Pt(II) complexes of the type [PtCl2L2] have a higher thermal stability than the corresponding Pt(0) complexes of the type [PtLn], with the exception of [Pt(SbPh3)3], which is more stable than [PtCl2(SbPh3)2]. Thermal stabilities of each of the complexes are compared with those of the others in the series. Mechanisms of thermal decomposition of complexes of the types [PtCl2L2] and [PtLn] are proposed. Residues of the samples were characterized by chemical tests and IR spectroscopy. The residue from the thermal decomposition of [PtCl2L2] (L is PPh3, AsPh3) and [Pt(PPh3)4] is metallic platinum. For [Pt(AsPh3)4] the residue is a mixture of Pt and As, whereas for the complexes containing SbPh3 the residues are mixtures of Pt and Sb. In these cases, the proportional contents of Pt and As or Pt and Sb correspond to the stoichiometry of these elements in the respective complexes. The complexes {[Pt(SbPh3)3]2N2}, {[Pt(SbPh3)3]2C2} lose N2 or the ethynediyl group at 130-150°C and are transformed into [Pt(SbPh3)3]. © 1995.