Short-chain di-ureasil ormolytes doped with potassium triflate: Phase diagram and conductivity behavior

Di-urea cross-linked poly(oxyethylene)/siloxane hybrids, synthesized by the sol-gel process and containing a wide concentration range of potassium triflate, KCF3SO3, have been analyzed by x-ray diffraction and differential scanning calorimetry. The pseudo-phase diagram proposed has been taken into account in the interpretation of the complex impedance measurements. The xerogels prepared are obtained as transparent, thin monoliths. At room temperature the highest conductivity found was 2 × 10-6 Ω-1 cm-1.

Influence of the processing conditions and corona poling on the morphology of β-PVDF

The α → β phase transformation of PVDF through the stretching process at different temperatures was investigated. The optimum stretching conditions were studied and characterised by infrared spectroscopy and differential scanning calorimetry. The maximum β-phase content was achieved at 80°C and a stretch ratio of 5. These samples were poled at several electric fields by the corona charge method. The effect of the electric field on the phase transformation was studied by infrared spectroscopy.

Inclusion complex of S(-) bupivacaine and 2-hydroxypropyl- β-cyclodextrin: Study of morphology and cytotoxicity

Local anesthetics (LA) belong to a class of pharmacological compounds that attenuate or eliminate pain by binding to the sodium channel of excitable membranes, blocking the influx of sodium ions and the propagation of the nerve impulse. S (-) bupivacaine (S(-) bvc) is a local anesthetic of amino-amide type, widely used in surgery and obstetrics for sustained peripheral and central nerve blockade. This article focuses on the characterization of an inclusion complex of S(-) bvc in 2-hydroxypropyl-β-cyclodextrin (HP-β-CD). Differential scanning calorimetry, scanning electron microscopy and X-Ray diffraction analysis showed structural changes in the complex. In preliminary toxicity studies, the cell viability tests revealed that the inclusion complex decreased the toxic effect (p<0.001) produced by S(-) bvc. These results suggest that the S(-) bvc:HP-β-CD inclusion complex represents a promising agent for the treatment of regional pain.

Methanol oxidation on PtRu/C electrocatalysts prepared by a microemulsion method

PtRu/C nanocatalysts were prepared by a microemulsion method using different values of water/surfactant molar ratio in order to get different particle sizes. Crystallite sizes and structural properties were determined by X-ray diffraction. Particle size and distribution were characterized by transmission electron microscopy and average composition was determined by energy dispersive X-ray analysis. Differential scanning calorimetry measurements indicated the presence of oxides in the as-prepared catalysts. The general electrochemical behavior was evaluated by cyclic voltammetry in 0.5 M sulfuric acid and the electrocatalytic activity towards the oxidation of methanol was studied in 0.5 M methanol acid solutions by potential sweeps and chronoamperometry. copyright The Electrochemical Society.

Protocolo para ensaios físico-químicos de estabilidade de fitocosméticos

The growing demand for stable, safe and effective cosmetics has required increasingly complex studies by the scientific community and the use of more efficient techniques to determine the stability of these products. The use of active principles from the Brazilian flora has led to the development of numerous products, in the most varied pharmaceutical forms, making it, even more difficult to standardize experimental protocols to certify the stability of cosmetic preparations. While in Brazil there is no one protocol that standardizes the tests that should be carried out to determine product stability, several studies have been conducted in academic laboratories to determine the stability of specific raw materials. The rheological properties of topical use products have to be taken into account in their manufacture, storage and application. The determination of the rheological behavior of a formulation helps in evaluating the physicochemical nature of the vehicle, allowing early signs of physical instability to be detected and thus enabling quality control of the constituents, test formulations and final products. Thermal analysis has also been used to assist in the study of cosmetic stability and differential scanning calorimetry to guide the development of new products. Other tools, such as fluorimetry and laser granulometry can be used to help the study and development of both emulsified and non-emulsified systems. The aim of the present study is to develop a protocol for the investigation of the physical and chemical stability of phytocosmetics - systems containing active compounds extracted from the Brazilian biodiversity.

Analytical model for heterogeneous crystallization kinetics of spherical glass particles

An analytical model developed to describe the crystallization kinetics of spherical glass particles has been derived in this work. A continuous phase transition from three-dimensional (3D)-like to 1D-like crystal growth has been considered and a procedure for the quantitative evaluation of the critical time for this 3D-1D transition is proposed. This model also allows straightforward determination of the density of surface nucleation sites on glass powders using differential scanning calorimetry data obtained under different thermal conditions. © 2009 The American Ceramic Society.

Synthesis, characterization and thermal study of solid mandelate of some bivalent transition metal ions in CO2 and N2 atmospheres

Solid state M-L, where M stands for bivalent transition metals (Mn(II), Fe(II), Co(II), Ni(II), Cu(II) and Zn(II)) and L is mandelate, were synthesized. Simultaneous thermogravimetry and differential scanning calorimetry, elemental analysis and complexometry were used to establish the stoichiometry and to study the thermal behaviour of these compounds in CO2 and N2 atmospheres. The results show that all the compounds were obtained in the anhydrous state and in agreement with the general formula ML2. The thermal decomposition of the compounds occurs in a single (Cu(II)), two (Ni(II)) three (Fe(II), Co(II)), four (Mn(II)) and five (Zn(II)) steps. The results also provided information concerning the ligand's denticity, thermal behaviour, final residues and identification of gaseous products evolved during the thermal decomposition of these compounds. © 2012 Akadémiai Kiadó, Budapest, Hungary.

Thermal behavior of lignin and cellulose from waste composting process

The lignin and cellulose were extracted from reference material (leaves and twigs) and food of compost at different times composting: zero (raw), 30, and 120 days. According to thermogravimetric analysis and its derivative and differential scanning calorimetry curves for these samples, were verified during composting process there were considerable changes in its thermal profiles, as well as, characteristics lignin in cellulose samples and cellulose in lignin samples. These features were found by fourier transformed infrared spectroscopy. © 2012 Akadémiai Kiadó, Budapest, Hungary.

The role of Bi2O3 on the thermal, structural, and optical properties of tungsten-phosphate glasses

Glasses in the ternary system (70 - x)NaPO3-30WO 3-xBi2O3, with x = 0-30 mol %, were prepared by the conventional melt-quenching technique. X-ray diffraction (XRD) measurements were performed to confirm the noncrystalline nature of the samples. The influence of the Bi2O3 on the thermal, structural, and optical properties was investigated. Differential scanning calorimetry analysis showed that the glass transition temperature, Tg, increases from 405 to 440 C for 0 ≤ x ≤ 15 mol % and decreases to 417 C for x = 30 mol %. The thermal stability against devitrification decreases from 156 to 67 C with the increase of the Bi2O3 content. The structural modifications were studied by Raman scattering, showing a bismuth insertion into the phosphate chains by Bi-O-P linkage. Furthermore, up to 15 mol % of Bi 2O3 formation of BiO6 clusters is observed, associated with Bi-O-Bi linkage, resulting in a progressive break of the linear phosphate chains that leads to orthophosphate Q0 units. The linear refractive index, n0, was measured using the prism-coupler technique at 532, 633, and 1550 nm, whereas the nonlinear (NL) refractive index, n 2 was measured at 1064 nm using the Z-scan technique. Values of 1.58 ≤ n0 ≤ 1.88, n2 ≥ 10-15 cm 2/W and NL absorption coefficient, α2 ≤ 0.01 cm/GW, were determined. The linear and NL refractive indices increase with the increase of the Bi2O3 concentration. The large values of n0 and n2, as well as the very small α2, indicate that these materials have large potential for all-optical switching applications in the near-infrared. © 2012 American Chemical Society.

Effect of Ag addition on phase transitions of the Cu-22.26 at.%Al-9.93 at.%Mn alloy

The phase transitions that occur in the Cu-22.26 at.%Al-9.93 at.%Mn and Cu-22.49 at.%Al-10.01 at.%Mn-1.53 at.%Ag alloys after slow cooling were studied using differential scanning calorimetry at different heating rates, microhardness changes with temperature, magnetization changes with temperature, scanning electron microscopy and energy dispersion X-ray spectroscopy. The results indicated that the presence of Ag does not modify the transition sequence of Cu-Al-Mn alloy, introduces a new transition due to the (Ag-Cu)-rich precipitates dissolution at about 800 K, and changes the mechanism of DO 3 phase dissolution. This mechanistic change was analyzed and a sequence of phase transitions was proposed for the reaction. © 2013 Elsevier B.V.

Thermal, rheological, and structural behaviors of natural and modified cassava starch granules, with sodium hypochlorite solutions

The use of chemically modified starches is widely accepted in various industries, with several applications. In this research, natural cassava starch granules were treated with standard sodium hypochlorite solution at 0.8, 2.0, and 5.0 g Cl/100 g starch. The native and modified starch samples were investigated by means of the following techniques: simultaneous thermogravimetry-differential thermal analysis, which allowed us to verify the thermal decomposition associated with endothermic or exothermic phenomena; and differential scanning calorimetry that was used to determine gelatinization enthalpy as well as the rapid viscoamylographic analysis that provided the pasting temperature and viscosity. By means of non-contact-atomic force microscopy method and X-ray powder patterns diffractometry, it was possible to observe the surface morphology, topography of starch granules, and alterations in the granules' crystallinity. © 2012 Akadémiai Kiadó, Budapest, Hungary.

Thermoanalytical study of nimesulide and their recrystallization products obtained from solutions of several alcohols

Thermogravimetry, differential scanning calorimetry, and vibrational infrared spectroscopy were used to study nimesulide and its recrystallization products that were obtained from solutions of several alcohols. The thermoanalytical measurements were performed in both air and nitrogen atmospheres and the results suggest that, under the experimental conditions used in this paper, it was possible to obtain neither polymorphic nor pseudopolymorphic forms of this drug. In this investigation, quantum chemical approach methods were used to determine the molecular structures using the Becke three-parameter hybrid method and the Lee-Yang-Parr correlation functional. The performed molecular calculations were done with the Gaussian 09 routine and the theoretical calculation results were correlated with the experimental IR vibrational spectrum. © 2013 Akadémiai Kiadó, Budapest, Hungary.

Study of the thermal behavior of bicuíba oil (Virola bicuhyba)

Bicuíba belongs to the Virola bicuhyba (Schott ex Spreng.) Warb species, Miristicaceas (Myristicaceae) family, which is frequently found in the Atlantic Forest of South and Southeast Brazil. Extraction of the Bicuíba oil was carried out and characterized by gas chromatography. The composition of in nature of this oil indicates that there is a predominance of saturated fatty acids with ~35 % lauric acid and ~40 % myristic acid. Details concerning the thermal behavior were evaluated by thermogravimetry, differential thermal analysis, and differential scanning calorimetry under oxygen and nitrogen atmospheres, showing thermal stability between 208 and 210 °C, respectively. Additionally, the kinetic studies were evaluated from several heating rates with a sample mass of 5 and 20 mg in open crucibles. The obtained data were evaluated with the isoconversional method kinetic, where the values of activation energy (Ea/kJ mol-1) were plotted in function of the conversion degree (α). © 2013 Akadémiai Kiadó, Budapest, Hungary.

Carbon nanotubes/polyamide 6.6 nanostructured composites crystallization kinetic study

Compared with the traditional composites, the incorporation of carbon nanotubes into polymeric matrices can generate materials with superior properties, especially thermal, electrical and tribological properties. The aim of this study was to study the polyamide 6.6/carbon nanotubes (PA 6.6/CNT) nanostructured composites crystallization kinetics. The solution mixing technique was used to obtain the nanostructured composites studied in this work. PA 6.6 films were produced with amounts of 0.1, 0.5, and 1.0 wt% (weight/weight) CNT. X-ray diffraction analyses were performed in order to determine the crystallographic properties of nanostructured composite. The nanostructured composites crystallization kinetic study was performed using the differential scanning calorimetry under isothermal and nonisothermal (dynamic) conditions. The results have shown addition of CNTs in the PA 6.6 reduces the Avrami exponent, affecting the crystallization process of the composite. © The Author(s) 2012.

RBPI21 interacts with negative membranes endothermically promoting the formation of rigid multilamellar structures

rBPI21 belongs to the antimicrobial peptide and protein (AMP) family. It has high affinity for lipopolysaccharide (LPS), acting mainly against Gram-negative bacteria. This work intends to elucidate the mechanism of action of rBPI21 at the membrane level. Using isothermal titration calorimetry, we observed that rBPI21 interaction occurs only with negatively charged membranes (mimicking bacterial membranes) and is entropically driven. Differential scanning calorimetry shows that membrane interaction with rBPI21 is followed by an increase of rigidity on negatively charged membrane, which is corroborated by small angle X-ray scattering (SAXS). Additionally, SAXS data reveal that rBPI21 promotes the multilamellarization of negatively charged membranes. The results support the proposed model for rBPI21 action: first it may interact with LPS at the bacterial surface. This entropic interaction could cause the release of ions that maintain the packed structure of LPS, ensuring peptide penetration. Then, rBPI21 may interact with the negatively charged leaflets of the outer and inner membranes, promoting the interaction between the two bacterial membranes, ultimately leading to cell death. © 2013 Elsevier B.V.