42 resultados para Solid state reaction method


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Solid state M-L compounds, where M stands for bivalent Mn, Ni, Cu and L is 4-methoxybenzoate, have been synthesized. Simultaneous thermogravimetry - differential thermal analysis (TG-DTA), X-ray powder diffractometry, infrared spectroscopy, elemental analysis and complexometry were used to characterize and to study the thermal behaviour of these compounds. The results led to information about the composition, dehydration, thermal stability and thermal decomposition of the isolated compounds.

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Solid state compounds of 4-methylbenzylidenepyruvate with Al(III), Ga(III), In(III) and Sc(III) have been synthesized. Complexometry, X-ray powder diffractometry, infrared spectroscopy and simultaneous thermogravimetry-differential thermal analysis (TG-DTA) have been used to characterize and to study the thermal behavior of these compounds. The results provided information concerning the stoichiometry, crystallinity, thermal stability and thermal decomposition of these compounds.

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Solid-state M-2-MeO-Bz compounds, where M stands for bivalent Mn, Co, Ni, Cu and Zn and 2-MeO-Bz is 2-methoxybenzoate, have been synthesized. Simultaneous thermogravimetry-differential thermal analysis (TG-DTA), thermogravimetry, derivative thermogravimetry (TG/DTG), differential scanning calorimetry (DSC), X-ray powder diffractometry, infrared spectroscopy and complexometry were used to characterize and to study the thermal behaviour of these compounds. The results led to have information about the composition, dehydration, thermal stability and thermal decomposition of the isolated compounds.

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Solid-state M-4-MeO-Bz compounds, where M stands for trivalent La, Ce, Pr, Nd and Sm and 4-MeO-Bz is 4-methoxybenzoate, have been synthesized. Simultaneous thermogravimetry and differential thermal analysis (TG-DTA), differential scanning calorimetry (DSC), X-ray powder diffractometry, infrared spectroscopy and complexometry were used to characterize and to study the thermal behaviour of these compounds. The results led to information about the composition, dehydration, polymorphic transformation, ligand's denticity, thermal behaviour and thermal decomposition of the isolated compounds.

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Solid-state Ln -3-MeO-Bz compounds, where Ln stands for lighter trivalent lanthanides (La Sm) and 3-methoxybenzoate, have been synthesized. Thermogravimetry (TG), differential scanning calorimetry (DSC), X-ray powder diffractometry, infrared spectroscopy, and complexometry were used to characterize and to study the thermal behaviour of these compounds. The results led to information concerning the composition, dehydration, polymorphic transformation, thermal behaviour and thermal decomposition of the synthesized compounds.

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Solid-state Ln-Bz compounds, where Ln stands for trivalent lanthanides and Bz is benzoate have been synthesized. Simultaneous thermogravimetric and differential thermal analysis in a CO2 atmosphere were used to study the thermal decomposition of these compounds.

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In this work, a protocol for the formulation of an enzyme concentrated product to be applied in fruit juice treatment is described. Downstream processing conditions for the recovery and concentration of pectinases produced by the new strain Aspergillus niger LB-02-SF in solid state cultivation were assessed. The solid-liquid ratio in the extraction step of pectinases recovery from the cultivated media was evaluated and the highest activity was obtained with a solid-liquid ratio of 1:10. The crude extract was concentrated by ultrafiltration and the total pectinase (TP) activity was 73.6-fold concentrated in relation to the crude extract, and a final TP titer of 663 U mL–1 was obtained with 73.7% of recovery yield. KCl and different glycerol concentrations were added to the concentrated extract and the stability of pectinases during the storage at 5°C for 59 weeks was tested. The formulation with 50% w/w glycerol was applied to the treatment of apple and grape juices and the results of these tests were statistically comparable to those obtained with two high-quality commercial preparations.

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Abstract The use of agroindustrial residues is an economical solution to industrial biotechnology. Coffee husk and pulp are abounding residues from coffee industry which can be used as substrates in solid state fermentation process, thus allowing a liberation and increase in the phenolic compound content with high added value. By employing statistical design, initial moisture content, pH value in the medium, and the incubation temperature were evaluated, in order to increase the polyphenol content in a process of solid state fermentation by Penicillium purpurogenum. The main phenolic compounds identified through HPLC in fermented coffee residue were chlorogenic acid, caffeic acid, and rutin. Data obtained through HPLC with the radical absorbance capacity assay suggest the fermented coffee husk and pulp extracts potential as a source of phenolic acids and flavonoids. Results showed good perspectives when using P. purpurogenum strain to enhance the liberation of phenolic compounds in coffee residues.

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Multicomponent ceramics are mainly synthesized by conventional solid-state reaction route and sol-gel routes. In the sol-gel route, colloidal or polymeric gel are envolved. In this work, some principles of the chemistry of theses routes are discused and it is ilustrated a variety of strategies for obtaining a homogeneous multicomponent precursors.

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Gadolinium oxyortho-silicate, Gd2SiO5, presents a monoclinic structure with two crystallographic sites in which Gd3+ ions are equally distributed with coordination numbers CN, 7 and 9, respectively. By doping this host with Er3+ it is possible to distinguish and attribute the two sites by means of lifetime determination of the 4S3/2 state, (in this case, Er3+ substitutes Gd3+ ions). Samples doped with 0.1 and 5.0% molar Er3+ were prepared by solid state reaction and characterized by X-ray Diffractometry, Vibrational and Electronic Absorption Spectroscopies, and Time Resolved Photoluminescence. Based on the experimental results, it is possible to verify that, for the 5,0% doped sample, the lifetime value of the 4S3/2 state of the erbium ion inserted in site 1, (CN = 9), is 2.7 ± 0.1 mus, and for the one inserted in site 2, (CN = 7), it is 1.5 ± 0.1 mus.

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The definition of a biomarker provided by the World Health Organization is any substance, structure, or process that can be measured in the body, or its products and influence, or predict the incidence or outcome of disease. Currently, the lack of prognosis and progression markers for chronic Chagas disease has posed limitations for testing new drugs to treat this neglected disease. Several molecules and techniques to detect biomarkers inTrypanosoma cruzi-infected patients have been proposed to assess whether specific treatment with benznidazole or nifurtimox is effective. Isolated proteins or protein groups from different T. cruzistages and parasite-derived glycoproteins and synthetic neoglycoconjugates have been demonstrated to be useful for this purpose, as have nucleic acid amplification techniques. The amplification of T. cruziDNA using the real-time polymerase chain reaction method is the leading test for assessing responses to treatment in a short period of time. Biochemical biomarkers have been tested early after specific treatment. Cytokines and surface markers represent promising molecules for the characterisation of host cellular responses, but need to be further assessed.

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Complexation between acyclovir (ACV), an antiviral drug used for the treatment of herpes simplex virus infection, and beta-cyclodextrin (beta-CD) was studied in solution and in solid states. Complexation in solution was evaluated using solubility studies and nuclear magnetic resonance spectroscopy (¹H-NMR). In the solid state, X-ray diffraction, differential scanning calorimetry (DSC), thermal gravimetric analysis (TGA) and dissolution studies were used. Solubility studies suggested the existence of a 1:1 complex between ACV and beta-CD. ¹H-NMR spectroscopy studies showed that the complex formed occurs with a stoichiometry ratio of 1:1. Powder X-ray diffraction indicated that ACV exists in a semicrystalline state in the complexed form with beta-CD. DSC studies showed the existence of a complex of ACV with beta-CD. The TGA studies confirmed the DSC results of the complex. Solubility of ACV in solid complexes was studied by the dissolution method and it was found to be much more soluble than the uncomplexed drug.

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This study investigated the content of total phenolic compounds and antioxidant activity in fermented rice bran in order to evaluate the effect of solid state fermentation on these properties. The process was performed with the fungus Rhizopus oryzae CTT 1217 in tray reactors at 30 °C for 120 hours. Samples of fermented rice bran were collected every 24 hours. Antioxidant property was evaluated by the diphenyl-1-picrylhydrazyl radical scavenging method and through the inhibition of enzymatic oxidation and lipid peroxidation of olive oil. The methanol extract of the biomass obtained at 96 hours of fermentation inactivated 50% of free radical in 15 minutes. The same extract reduced the peroxide value in the olive oil by 57% after 30 days of storage. The aqueous extract of the biomass obtained at 120 hours was the most efficient inhibitor of the darkening reaction catalyzed by peroxidase.

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Single-stranded DNA (ssDNA) is a prerequisite for electrochemical sensor-based detection of parasite DNA and other diagnostic applications. To achieve this detection, an asymmetric polymerase chain reaction method was optimised. This method facilitates amplification of ssDNA from the human lymphatic filarial parasite Wuchereria bancrofti. This procedure produced ssDNA fragments of 188 bp in a single step when primer pairs (forward and reverse) were used at a 100:1 molar ratio in the presence of double-stranded template DNA. The ssDNA thus produced was suitable for immobilisation as probe onto the surface of an Indium tin oxide electrode and hybridisation in a system for sequence-specific electrochemical detection of W. bancrofti. The hybridisation of the ssDNA probe and target ssDNA led to considerable decreases in both the anodic and the cathodic currents of the system's redox couple compared with the unhybridised DNA and could be detected via cyclic voltammetry. This method is reproducible and avoids many of the difficulties encountered by conventional methods of filarial parasite DNA detection; thus, it has potential in xenomonitoring.

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Rare earth elements supported in zeolites are the most important catalysts in the fluid cracking of petroleum. The solid state ion exchange of Eu3+ in Y zeolite was investigated. First of all, the hydrated EuCl3 was well mixed in a ball mill and was then heated at 300ºC for different times. The quantitative determination of Eu3+ showed that the degree of ion exchange depends on the reaction time at constant temperature, being ~95% in 4 h. The X-ray study showed that the crystallinity of the zeolite is little affected by the exchange procedure. The study of spectroscopic properties of Eu3+, emission spectra and lifetime, give information about the migration and position of the ion in the zeolite cages.