Caracterização e propriedades catalíticas da zeolita HZSM5 modificada com nióbio

HZSM5 zeolite was modified by exchanging proton by niobium (V). Several samples were obtained with various degrees of exchange. Pore volumes and acidity were measured to characterize these exchanged zeolites. Catalytic properties were evaluated with two reaction tests: m-xylene transformation and n-heptane cracking. The introduction of niobium on HZSM5 zeolite decreases the diffusion coefficient of 2-methyl-pentane and increases the zeolite acidity. The sample containing niobium are initially more active in cracking of n-heptane and m-xylene isomerization than HZSM5 alone.

Síntese e caracterização estrutural de complexos mono e bimetálicos de paládio e platina com ligantes contendo nitrogênio e enxofre

The synthesis of several mono- and bimetallic platinum and palladium complexes are reported. The monometallic complexes are of the type MCl2(PEt3)2L (L=2-aminothiazol; benzothiazol; 2-imidazolidithione; M=Pt; Pd), and the bimetallic complexes (M2Cl4(PEt3) 2L) are derived from them. Infrared spectroscopic characterization of the monometallic complexes shows that the metal centre are coordinated through the N-endocyclic (L=2-aminothiazol; benzothiazol) and through the sulphur when L=2-imidazolidithione. Coordination of a second metal fragment occurs via the sulphur atom (L=2-aminothiazol; benzothiazol) according to infrared studies. 31P{¹H} NMR spectroscopy suggest that the complexes have a cis- configuration since the ¹J Pt-P are around the value found for this type of compound.

Compósitos colágeno aniônico: fosfato de cálcio. Preparação e caracterização

Anionic collagen: calcium phosphate composite was obtained by controlled mixing of collagen and calcium phosphate until the consistence of a past. Material was characterized by a Ca/P ratio of 1.55, with a X-ray diffraction pattern similar to that for hydroxyapatite. Differential Scanning Calorimetry showed that the protein is not denatured under the processing conditions. Scanning Electronic Microscopy showed that the mineral phase are regularly covered with collagen fibers, indicating that anionic collagen is efficient in the preparation of stable form of calcium phosphate ceramic paste.

Preparação e caracterização de eletrodos monocristalinos

Studies of the kinetics of electrocatalytic reactions on well oriented single crystal surfaces have demonstrated the influence of surface structure on the rate and mechanisms of many electrochemical processes. The preparation and characterization of these surfaces is the first step in this type of studies. In this paper, a methodology employed in order to ensure the quality and cleanliness of single crystals and their utilization as rotating electrodes is described.

Desenvolvimento e caracterização de recobrimentos de Ni-Co e de seus óxidos mistos para a produção de oxigênio por eletrólise alcalina da água

This paper describes the development and characterisation of Ni-Co coatings to be used as anodes in water electrolysis. Chemical oxidation of the surface was performed through thermal treatment at 400ºC for 10 h. The resulting surfaces were analysed by X-ray diffraction, EDX, SEM, cyclic voltammetry and constant current electrolysis. The electrochemical oxidation occurring on bare surfaces during electrolysis promotes the formation of thick oxide layers resulting in loss of activity. In oxidised surfaces the chemical Ni-Co oxide grown during the thermal treatment prevents further oxidation thus retaining their activity towards oxygen evolution. An optimum condition for the growth of mixed oxide with high activity was found for the bath containing 50 g L-1 CoSO4.

Preparo de óxido de nióbio suportado em alumina por deposição química em fase vapor: caracterização por espectroscopia vibracional e termogravimetria

Alumina supported niobium oxide was prepared by chemical vapor deposition (CVD) of NbCl5. The alumina was calcined and pretreated at differents temperatures in order to vary the density of OH groups on the surface which was determined by thermogravimetric analysis. A good correlation was found between the amount of anchored niobium and the total number of anionic sites (oxide and hydroxyl groups) on the surface of the alumina. The infrared spectra on the OH stretching region indicate that OH groups coordinated to at least one tetrahedral aluminum were more reactive towards NbCl5.

Hidrólise seletiva de carboxiamidas de resíduos de asparagina e glutamina em colágeno: preparação e caracterização de matrizes aniônicas para uso como biomateriais

This work describes the selective hydrolysis of carboxyamide groups of asparagine and glutamine of collagen matrices for the preparation of negatively charged collagen biomaterials. The reaction was performed in the presence of chloride and sulfate salts of alkaline and alkaline earth metals in aqueous dimethylsulfoxide solution and, selectively hydrolysis of carboxyamide groups of collagen matrices was promoted without cleavage of the peptide bond. The result is a new collagen material with controlled increase in negative charge content. Although triple helix secondary structure of tropocollagen was preserved, significative changes in thermal stabilities were observed in association with a new pattern of tropocollagen macromolecular association, particularly in respect microfibril assembly, thus providing at physiological pH a new type of collagen structure for biomaterial preparation, characterized by different charge and structural contents .

Caracterização química e física de vermicomposto e avaliação de sua capacidade em adsorver cobre e zinco

The physical and chemical characterization of vermicompost from bovine manure has been studied. It was examined the pH and cation exchangeable capacity (CEC), organic matter content, electric conductivity and elementary and XRD analyses, among other characteristics. The vermicompost was then applied to the retention and competition of metal micronutrients and pollutants (Cu and Zn) from metal nitrate solutions. The retention was affected by both the pH and adsorption time, while the competitive character of these metals for the substrate was relevant to each pH examined.

Sistema com atmosfera controlada para a caracterização de sensores a gases

This paper describes a sample holder for the electrical measurement of oxides or conducting polymers in the form of pellets or films which are used as gas sensors. The system makes it possible to control the sample temperature, the gas pressure and composition. The temperature in the sample can be changed from 25ºC to 450ºC, and the gas pressure in the chamber is controlled between 5 ¥ 10-4 and 1000 mbar. The performance of the system in resistance measurements of doped tin oxide pellets and polyaniline films deposited on platinum electrodes for methane is analyzed.

Caracterização de filmes finos de Nb2O5 com propriedades eletrocrômicas

The sols for thin electrochromic coatings of Nb2O5 were obtained by synthesis of the niobium butoxide from BuONa and NbCl5. The ~300nm thick films were deposited by dip-coating technique from the alkoxide solution and calcined at 560ºC in O2 atmosphere during 3 hours. The particles size of niobium oxide (V) powder (~20mm) was obtained from x-ray diffraction using the Scherrer equation. The coatings were characterized by cyclic voltammetry and cronoamperommetry techniques. The spectral variation of the optical transmittance were determined in situ as a function of the cyclical potencial and memory effect. The insertion process of lithium is reversible and change the film color from transparent (T=80%) to dark blue (T=20%).

Nova rota de preparação do 2-cloro-1,3,2-dioxofosfolana e 2-cloro-4,5-benzo-1,3,2-dioxofosfolana e caracterização por espectroscopia de RMN multinuclear

A new method for the preparation of 2-chloro-1,3,2-dioxaphospholane (1) and 2-chloro-4,5-benzo-1,3,2-dioxaphospholane (2), are reported. The modifications introduced in the synthetic route improved the yield and facilitated the control of reaction, but the synthesis require longer reaction time. The compounds were characterized by ¹H, 13C{¹H} and31P{¹H} NMR spectroscopy. Due to the complexity of the spin system AA'BB'X (A, A', B, B' = ¹H; X = 31P) of 2, a simulation of the ¹H NMR spectra was done and it's in agreement with the bibliography.

Metais pesados em águas superficiais como estratégia de caracterização de bacias hidrográficas

The input of heavy metals concentrations determinated by ICP-AES, in samples of the Cambé river basin, was evaluated by using the Principal Component Analysis. The results distinguishes clearly one site, which is strongly influenced by almost all elements studied. Special attention was given to Pb, because of the presence of one battery industry in this area. Some downstream samples were associated with the same characteristics of this site, showing residual action of contaminants along the basin. Other sites presented influence of soil elements, plus Cr near a tannery industry. This study allowed to distinguish different sites in the upper basin of the Cambé (Londrina-PR-BR), in accordance to elements input.