Solid-state LnL3∙nH2O complexes, where Ln stands for trivalent lanthanides (Tb to Lu) or yttrium(III) and L is oxamate (NH2COCO2-), have been synthesized. The characterization of the complexes was performed by using elemental analysis (EA), complexometric titration with EDTA, thermoanalytical techniques such as simultaneous thermogravimetry and differential scanning calorimetry (TG-DSC), evolved gas analysis (TG-FTIR), infrared spectroscopy (IR) and powder X-ray diffraction (XRPD). The results provided information about thermal behavior, crystallinity, stoichiometry, coordination sites, as well as the products released during thermal degradation of the complexes studied. Theoretical calculation of yttrium oxamate, as representative of all complexes was performed using density functional theory (DFT) for studying the molecular structure and vibrational spectrum of the investigated molecule in the ground state. The optimized geometrical parameters and theoretical vibrational spectrum obtained by DFT calculations are in good agreement with the experimental results.

Foram preparadas suspensões de TiO2 dopadas com Fe(III) pelo método sol-gel. As propriedades dos materiais dopados foram comparadas com a de TiO2 puro, baseadas na caracterização por análise térmica (TG-DTA e DSC), difratometria de raios X e medidas espectroscópicas (FTIR). As suspensões de TiO2 puras e dopadas foram depositadas sobre substrato metálico, obtendo-se assim eletrodos de filme fino. O tratamento térmico destes precursors a 400 ºC por um período de 2 horas resultou na formação de fase cristalina anatase. Os eletrodos foram utilizados em processo fotoeletrocatalítico para a degradação de corante têxtil em solução aquosa. Verificou-se que o eletrodo de TiO2 puro apresentou melhor desempenho no processo de degradação do corante.

Pure and Fe(III)-doped TiO2 suspensions were prepared by the sol gel method with the use of titanium isopropoxide (Ti(OPri)4) as precursor material. The properties of doped materials were compared to TiO2 properties based on the characterization by thermal analysis (TG-DTA and DSC), X-ray powder diffractometry and spectroscopy measurements (FTIR). Both undoped and doped TiO2 suspensions were used to coat metallic substrate as a mean to make thin-film electrodes. Thermal treatment of the precursors at 400ºC for 2 h in air resulted in the formation of nanocrystalline anatase TiO2. The thin-film electrodes were tested with respect to their photocatalytic performance for degradation of a textile dye in aqueous solution. The plain TiO2 remains as the best catalyst at the conditions used in this report.

Several papers have been described on the thermal stability of the sweetener, C12H19Cl3O8 (Sucralose). Nevertheless no study using thermoanalytical techniques was found in the literature. Simultaneous thermogravimetry and differential thermal analysis (TG-DTA), differential scanning calorimetry (DSC) and infrared spectroscopy, have been used to study the thermal stability and thermal decomposition of sweetener.

Estudos potenciométricos foram realizados para determinar o grau de ligação do ácido fítico com os íons Co(II) e o Mn(II), na ausência de dioxigênio. As constantes de equilíbrio para as principais espécies formadas são relatadas, e os resultados são representados na forma de diagramas de distribuição mostrando a concentração individual dos complexos como uma função do pH. Os valores das constantes de formação dos complexos foram elevados para as espécies em que o ligante encontra-se mais desprotonado. Os dados potenciométricos indicam que a espécie [MH4L]6-, encontra-se totalmente formada em pH 7,0 e a partir destes dados os complexos de Mn(II) e Co(II) com o ácido fítico foram sintetizados no estado sólido. Análises de infravermelho, termogravimetria e calorimetria exploratória diferencial foram utilizadas para caracterizar e investigar o comportamento térmico destes compostos. Os resultados conduziram a informações sobre composição, desidratação, estabilidade e decomposição térmica dos complexos.

Potentiometric studies were carried out to determine the binding degree of phytic acid with Co(II) and Mn(II) ions, in the absence of dioxygen. Equilibrium constants for all major complexes formed are reported, and the results are presented in the form of distribution diagrams showing the concentrations of individual complexes as a function of pH. The formation constants of the complexes show higher values for the species in which the ligand was more deprotonated. Potentiometric data indicates that the species [MH4L]6-, was totally formed at pH 7.0 and the complexes were synthesized from this data. A solid state complex of Mn(II) and Co(II) with phytic acid was synthesized. Thermogravimetry, differential scanning calorimetry, and infrared spectroscopy were used to investigate and characterize the thermal behavior of these compounds. The results led to information on the composition, dehydration, thermal stability and thermal decomposition of the isolated complexes.

A rapid, sensitive and reliable thin-layer chromatography/spectrophotometry screening procedure was developed for quantitative determination of diuretics associated in pharmaceutical dosage forms. The chromatographic method employed microcrystalline cellulose and butanol : acetic acid : water (4:1:1) or amilic alcohol : ammonium hydroxide 25% (9:1) as mobile phases and detection by U.V. light. The drugs were extracted using a simple procedure and were quantified by U.V. spectrophotometry. Results varied from 97.5 to 102.5% and are similar to those obtained by conventional methods. This method of quantification of diuretics is promising for quality control of drugs.

Solid-state MBz compounds, where M stands for bivalent Mn, Fe, Co, Ni, Cu and Zn and Bz is benzoate, have been synthesized. Simultaneous thermogravimetry and differential thermal analysis (TG-DTA), differential scanning calorimetry (DSC), infrared spectroscopy and complexometry were used to characterize and to study the thermal behaviour of these compounds. The procedure used in the preparation of the compounds via reaction of basic carbonates with benzoic acid is not efficient in eliminating excess acid. However the TG-DTA curves permitted to verify that the binary compounds can be obtained by thermosynthesis, because the benzoic acid can be eliminated before the thermal decomposition of these compounds. The results led to information about the composition, dehydration, thermal stability, thermal decomposition and structure of the isolated compounds. On heating, these compounds decompose in two (Mn, Co, Ni, Zn) or three (Fe, Cu) steps with formation of the respective oxide (Mn3O4, Fe2O3, Co3O4, NiO, CuO and ZnO) as final residue. The theoretical and experimental spectroscopic studies suggest a covalent bidentate bond between ligand and metallic center.

Os compostos dos 4-dimetilaminocinamalpyruvatos (4-DMCP) de Mn (II), Co (II), Ni (II), Cu (II), Zn (II) e Pb (II) foram preparados. Estes compostos foram estudados pelas técnicas termoanaliticas: termogravimetria (TG), termogravimetria derivada (DTG), calorimetria exploratória diferencial (DSC), difratometria de raios - X pelo método do pó e titulação complexométrica com EDTA. Através dos resultados obtidos pela titulação complexométrica com EDTA, TG, DTG e DSC foi possível estabelecer o grau de hidratação, estequiometria e estabilidade térmica dos compostos preparados.

Solid state compounds M-4-DMCP, where 4-DMCP is 4-dimethylaminocinnamylidenepyruvate and M represents Mn (II), Co (II), Ni (II), Cu (II), Zn (II) and Pb (II) were prepared. These compounds were studied by thermoanalitycal techniques: thermogravimetry (TG), derivative thermogravimetry (DTG), differential scanning calorimetry (DSC), X-ray diffraction powder patterns and complexometric titration with EDTA. From the results obtained by the complexometric titration with EDTA, TG, DTG and DSC curves, was possible to establish the hydration degree, stoichiometry and thermal stability of the prepared compounds.

Os cinamalpiruvatos de lantanídeos (III) (exceto promécio) e de ítrio (III), foram preparados no estado sólido. A termogravimetria, termogravimetria derivada (TG, DTG), calorimetria exploratória diferencial (DSC), difratometria de raios X e complexometria foram utilizadas para caracterizar e estudar o comportamento térmico desses compostos em atmosfera dinâmica de CO2. Os resultados obtidos mostraram diferenças significativas na estabilidade e na decomposição térmica desses compostos em relação ao estudo do comportamento térmico em atmosfera dinâmica de ar.

Solid state cinnamylidenepyruvate of trivalent lanthanides (except for promethium) and yttrium, were prepared. Thermogravimetry, derivative thermogravimetry (TG, DTG), differential scanning calorimetry (DSC), X-ray diffraction powder patterns and complexometry were used to characterize and to study the thermal behavior of these compounds in a dynamic CO2 atmosphere. The results obtained showed significative differences on the thermal stability and thermal decomposition of these compounds, with regard to the thermal behavior study in a dynamic air atmosphere.

Óleos e gorduras vegetais são muito ultilizados pela indústria alimentícia e farmacêutica, tem exigido de pesquisadores e técnicos métodos analíticos capazes de avaliar as condições de processamento e estocagem. A estabilidade térmica de óleos vegetais é um fator determinante na sua qualidade. Neste trabalho avaliou-se a estabilidade térmica de óleos e gorduras vegetais extraídos de semente de plantas do cerrado ( araticum, babaçu, buriti, guariroba e murici) usando os resultados de TG, DTG e DTA, numa faixa de temperatura entre 30 e 650ºC, em atmosfera de nitrogênio, com razão de aquecimento de 10ºC min-1. As técnicas termoanalíticas utilizadas mostraram-se eficientes e rápidas na determinação da estabilidade térmica dos óleos e gorduras estudados.

Vegetal oils and fats are very useful in the food and chemist industry, they have demanded from researchers and technicians analytical methods able to estimate the conditions for their processing and storage. The thermal stability of vegetal oils is a main determinant in recognizing their value. The goal of this study is to evaluate the thermal stability of vegetable oils and fats extracted from the seeds of plants from Brazilian cerrado (araticum, babassu, Brazilian wine-palm, guariroba, murici). The thermal stability was evaluated by TG/DTG and DTA techniques, in a temperature range from 30º to 650º, under nitrogen atmosphere, and at a heating rate 10º C min-1. The TG/DTG and DTA used were efficient and fast in the determination of oils and fasts studied.

A calorimetria exploratória diferencial (DSC) foi utilizada na caracterização do acetato de dexametazona (princípio ativo), álcool cetílico, emulgin, polawax, nipagim-M (excipientes). O princípio ativo também foi investigado utilizando-se a termogravimetria (TG) e espectroscopia de absorção na região do ultravioleta e visível (UV-VIS). Os resultados obtidos permitiram verificar a estabilidade térmica e o ponto de fusão do princípio ativo, bem como o ponto de fusão dos excipientes utilizados na fabricação do creme de dexametazona.

Differencial scanning calorimetry (DSC) technique have been used to characterize the dexamethasone acetate (active component), cetyl alcohol, emulgin, polawax and nipagim-M (excipents). The active component have also been investigated by TG, DTG and ultraviolet and visible absorption spectra (UV-VIS). The results permitted us to verify the thermal stability and melting point of the active component, as well as the melting point of the excipients used to produce the dexamethasone cream.

Foram preparados no estado sólido, compostos de fórmula geral M(DMCP)2 nH2O, em que M representa Mg, Ca, Sr, Ba; DMCP é 4-dimetilaminocinamalpiruvato e n = 1, exceto para o Ca onde n = 2,5. Na caracterização, bem como no estudo da decomposição térmica desses compostos, foram utilizados a termogravimetria, termogravimetria derivada (TG, DTG), calorimetria exploratória diferencial (DSC), difração de raios-X pelo método do pó e complexometria.

Solid state compounds of general formula M(DMCP)2.nH2O, where M represents Mg, Ca, Sr, Ba, and DMCP is 4-dimethylaminocinnamylidenepyruvate, and n = 1, except for Ca, where n = 2.5, have been prepared. Thermogravimetry, derivative thermogravimetry (TG, DTG), differential scanning calorimetry (DSC), X-ray diffraction powder patterns and complexometry were used to characterize and to study the thermal decomposition of these compounds.

Foram preparados os ditizonatos de Hg (I), Ag (I) e Bi (III). Termogravimetria (TG), termogravimetria derivada (DTG), calorimetria exploratória diferencial (DSC), difratometria de raios X pelo método do pó e análise elementar foram usados para caracterizar e para estudar a estabilidade térmica e a decomposição térmica da ditizona e destes ditizonatos.

Solid dithizonates of Hg(I), Ag(I) and Bi(III) have been prepared. Thermogravimetry (TG), derivative thermogravimetry (DTG), differential scanning calorimetry (DSC), X ray diffraction powder patterns and elemental analysis have been used to characterize and to study the thermal stability and thermal decomposition of the dithizone and of these dithizonates.

Termogravimetria, termogravimetria derivada (TG,DTG), calorimetria exploratória diferencial (DSC) e difratometria de raios X foram utilizados para estudar o trimetroprim, sulfametoxazol, ampicilina, cloridrato de tetraciclina e rifampicina. Os resultados permitiram obter informações sobre a estabilidade térmica destes compostos e a decomposição térmica em atmosfera de ar.

Thermogravimetry, derivative thermogravimetry (TG, DTG), differential scanning calorimetry (DSC) and X ray diffraction powder patterns have been used to study trimethoprim, sulfamethoxazole, ampicillim, tetracycline hydrochloride and rifampim. The results revealed the extent of their thermal stability and also allowed interpretations concerning their thermal decompositions in air atmosphere.

Estudos termogravimétricos e calorimétricos diferenciais para ditiocarbamatos de NH4+, Na+, Zn2+, Cd2+ e Pb2+, derivados de aminas cíclicas contendo nitrogênio como heteroátomos, foram realizados em atmosferas de ar e nitrogênio, para avaliar a influência da tensão angular dos anéis na decomposição térmica destes compostos, em relação à formação de tiocianatos metálicos como via de decomposição. Os intemediários formados foram caracterizados por difração de raios-X, tendo sido encontrados oxissulfatos de Zn2+, Cd2+ e Pb2+, sob atmosfera de ar, o que sugere a decomposição térmica nestas condições como via sintética para estes compostos. Os produtos de decomposição final obtidos foram sulfetos metálicos sob nitrogênio e óxidos dos metais de transição e sulfato de sódio sob ar. Entalpias de fusão são também descritas, com base nos resultados de DSC.

Thermogravimetric and Differential Scanning Calorimetric investigation of the thermal behaviour of NH4+, Na+, Zn2+, Cd2+ e Pb2+ dithiocarbamates obtained from cyclic amines, is described under nitrogen and air atmospheres in order to investigate the effect of a cyclic ring on the mechanism of decomposition. Intermediates were identified by X-ray Diffraction analysis. Zn2+, Cd2+ e Pb2+ oxysulphates were detected under air atmosphere suggesting the thermal decomposition under these conditions as an alternating synthetic route to prepare those compounds. The final decomposition products were the metallic sulphides under N2 atmosphere while transition metal oxides and sodium sulphate were obtained under air. Melting enthalpies are also reported from DSC data.

Foram preparados compostos no estado sólido Ln-OHCO3-DMCP, onde Ln representa os íons lantanídios(III) e ítrio(III) e DMCP é o ion 4-dimetilaminocinamalpiruvato. Na caracterização, bem como no estudo da decomposição térmica desses compostos, foram utilizados as técnicas termoanalíticas (TG, DTG, DSC) difratometria de raios X e análise elementar. A estabilidade bem como a decomposição térmica foram estudadas em atmosfera de ar utilizando cadinho de alumina.

Solid Ln-OHCO3-DMCP compounds, where Ln represents lanthanides (III) and yttrium (III) ions and DMCP is the anion 4-dimethylaminocinnamylidenepyruvate, have been prepared. Thermogravimetry, derivative thermogravimetry (TG, DTG), differential scanning calorimetry (DSC), x-Ray diffraction powder patterns and elemental analysis have been used to characterize the compounds. The thermal stability as well as the thermal decomposition of these compounds were studied using an alumina crucible in an air atmosphere.