Preparation, thermal characterization, and DFT study of the bacterial cellulose

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

Facile synthesis and characterization of ZrO2 nanoparticles prepared by the AOP/hydrothermal route

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

Investigation of chemical changes in sealers during application of the warm vertical compaction technique

Aim To assess (i) heat generated by pluggers during warm vertical compaction of gutta-percha and investigation of temperature changes on the external root surface during canal filling, and (ii) the chemical changes of root canal sealers induced by heat.Methodology Four sealers, namely AH Plus, MTA Plus and two other experimental sealers based on tricalcium silicate, were characterised. External temperatures generated on the root surface during warm vertical compaction of gutta-percha with different sealers inside the root canal were monitored using an infrared thermography camera. Chemical changes induced by heating the sealers were assessed by Fourier transform infrared (FT-IR) spectroscopy.Results MTA Plus and the experimental sealers were composed of a cement and radiopacifier, with epoxy resin or a water-soluble polymer as dispersant, whilst AH Plus was epoxy resin-based. The heat generated at the tips of the continuous wave pluggers was found to be lower than the temperature set and indicated on the device LCD display. The sealers reduced the heat generated on the external root surfaces during the heating phase. AH Plus sustained changes to its chemical structure after exposure to heat, whilst the other sealers were unaffected.Conclusions The temperatures recorded at the tips of continuous wave pluggers varied with their taper and were lower than the temperature set on the System B LCD display. Root canal sealers reduced the dissipation of heat generated during warm vertical compaction, with the temperature at the external root surface maintained at 37-41 degrees C, a temperature below that is necessary to cause irreversible damage to bone and periodontium. The use of AH Plus sealer during warm vertical compaction techniques results in chemical changes in the sealer. The effect on sealer properties needs to be further investigated.

Estudo do potencial de associações de ZnO com os produtos naturais ácido cafeico e ferúlico como filtros solares híbridos: [recurso eletrônico]

In this work were studied associations of ZnO with the natural products caffeic and feluric acids. Two preparation methods were used, that is, the sol-gel and a reflux procedure. In the sol-gel method, ZnO is produced by the basics hydrolysis of precursors in the presence of the organic filters (caffeic and feluric acids), which results in 30 nm (or less) ZnO particles with the organic filters (in dissociated form) bonded to the surface of ZnO. In the reflux method, a dispersion of ZnO in a water/ethanol mixture was kept under reflux (50oC/4h) in the presence of the organic acids. The ZnO particles used in the reflux method have a higher diameter than sol-gel ZnO particles, but the prepared associated product ZnO/Organic acids were similar. Despite of the difference in relation to crystallinity between the products, the preparation methods resulted in analogous associations with respect to the interaction of the organic filters with the ZnO surface. The caffeic/ZnO associations presented low photostability, which lead to the degradation of the organic filter. The other associations (feluric acid/ZnO) presented satisfactory results. The FT-IR spectroscopy confirmed the formation of the association, and the nature of the bond formed compared with the Zn-O bond in Zn2+/Felutic acid complexes. The isolated organic and inorganic filters, along with the associations were analyzed by diffuse reflectance spectroscopy and Uv-vis spectroscopy. The absorption edges and the critical wavelengths were analyzed and the effects of Zn-O bonds in feluric acid/ZnO associations described as a function of the relative position of the π/π* system of the organic filter. Finally the performance of the hybrid filters were investigated in terms of the absorption of UVA and UVB radiations, with the UVA/UVB ratio, an efficiency parameter largely used in the description of solar filters, sunscreen and suncare products

Towards an understanding on the role of precursor in the synthesis of ZnS nanostructures

Wurtzite-structured ZnS nanostructures have been synthesized by means of a microwave-solvothermal method at 140°C using three precursors (chloride, nitrate and acetate). Different techniques such as X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), Fourier transform infrared (FT-IR) spectroscopy, ultraviolet–visible (UV–vis) absorption spectroscopy and photoluminescence (PL) measurements have been employed to characterize this material. The structure, surface morphology, chemical composition and optical properties were investigated as function of precursor. In order to complement experimental results, first principles calculations at DFT level were carried out in order to obtain the relative stability of the proposed intermediates along the formation mechanism. - See more at: http://www.eurekaselect.com/117237/article#sthash.GzvnCBTB.dpuf

Chemical characterization and bioactivity of epoxy resin and Portland cement-based sealers with niobium and zirconium oxide radiopacifiers

The purpose of this study was to characterize and to evaluate the bioactivity potential of experimental root canal sealers (ES) based on Portland cement, epoxy resin with nano- and micro-particles of niobium or zirconium oxide used as radiopacifiers in comparison to AH Plus and MTA Fillapex. Methods Specimens of the sealers (10 mm in diameter × 1 mm thick) were prepared and the radiopacity was evaluated according to ISO 6876 (2012) specifications. Characterization of the sealers was performed under the scanning electron microscope (SEM) immediately after setting and after immersion for 28 days in Hank's balanced salt solution (HBSS). In addition X-ray energy dispersive spectroscopy (EDS), X-ray diffraction (XRD) and Fourier transform infrared (FT-IR) spectroscopy were also performed. The pH and calcium ion release were measured after 1, 7, 14, 21 and 28 days after completion of seating using a digital pH meter and an atomic absorption spectrophotometer, respectively. Results The experimental sealers exhibited an average radiopacity of 2.5 mm thickness of aluminum, which was similar to MTA Fillapex (P > 0.05) and inferior to AH Plus (P < 0.05). AH Plus did not show bioactivity. Although the experimental sealers did not exhibit the formation of hydration product, they encouraged the deposition of crystalline spherical structures of calcium deficient phosphate. The highest pH and calcium release values were observed with the experimental sealers (P < 0.01). ES-Nb-micro was the only sealer to present hexagonal shaped crystal deposition. Significance Novel root canal sealers based on a mixture of Portland cement, epoxy resin and radiopacifier exhibited a degree of bioactivity although no evidence of cement hydration was demonstrated on material characterization. The radiopacifier particle size had limited effect on the sealer microstructure and chemical properties.

Effects of acetylation and acetylation-hydroxypropylation (dual-modification) on the properties of starch from Carioca bean (Phaseolus vulgaris L.)

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Influence of beta-cyclodextrin on the properties of norfloxacin form A

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

Rietveld refinement, cluster modelling, growth mechanism and photoluminescence properties of CaWO4: Eu3+ microcrystals

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

The filler content of the dental composite resins and their influence on different properties

The purpose of this study was to compare the inorganic content and morphology of one nanofilled and one nanohybrid composite with one universal microhybrid composite. The Vickers hardness, degree of conversion and scanning electron microscope of the materials light-cured using LED unit were also investigated. One nanofilled (Filtek (TM) Supreme XT), one nanohybrid (TPH (R) 3) and one universal microhybrid (Filtek (TM) Z-250) composite resins at color A2 were used in this study. The samples were made in a metallic mould (4 mm in diameter and 2 mm in thickness). Their filler weight content was measured by thermogravimetric analysis (TG). The morphology of the filler particles was determined using scanning electron microscope equipped with a field emission gun (SEM-FEG). Vickers hardness and degree of conversion using FT-IR spectroscopy were measured. Filtek (TM) Z-250 (microhybrid) composite resin shows higher degree of conversion and hardness than those of Filtek (TM) Supreme XT (nanofilled) and TPH (R) 3 (nanohybrid) composites, respectively. The TPH3 (R) (nanohybrid) composite exhibits by far the lowest mechanical property. Nanofilled composite resins show mechanical properties at least as good as those of universal hybrids and could thus be used for the same clinical indications as well as for anterior restorations due to their high aesthetic properties. Microsc. Res. Tech. 75:758765, 2012. (C) 2011 Wiley Periodicals, Inc

Structural refinement, optical and microwave dielectric properties of BaZrO3

In this work, barium zirconate (BaZrO3) ceramics synthesized by solid state reaction method and sintered at 1670 degrees C for 4 h were characterized by X-ray diffraction (XRD), Rietveld refinement, and Fourier transform infrared (FT-IR) spectroscopy. XRD patterns, Rietveld refinement data and FT-IR spectra which confirmed that BaZrO3 ceramics have a perovskite-type cubic structure. Optical properties were investigated by ultraviolet-visible (UV-vis) absorption and photoluminescence (PL) measurements. UV-vis absorption spectra suggested an indirect allowed transition with the existence of intermediary energy levels within the band gap. Intense visible green PL emission was observed in BaZrO3 ceramics upon excitation with a 350 nm wavelength. This behavior is due to a majority of deep defects within the band gap caused by symmetry breaking in octahedral [ZrO6] clusters in the lattice. The microwave dielectric constant and quality factor were measured using the method proposed by Hakki-Coleman. The dielectric resonator antenna (DRA) was investigated experimentally and numerically using a monopole antenna through an infinite ground plane and Ansoft's high frequency structure simulator software, respectively. The required resonance frequency and bandwidth of DRA were investigated by adjusting the dimension of the same material. (C) 2011 Elsevier Ltd and Techna Group S.r.l. All rights reserved.

Metal biosorption onto dry biomass of Arthrospira (Spirulina) platensis and Chlorella vulgaris: Multi-metal systems

Binary and ternary systems of Ni2+, Zn2+, and Pb2+ were investigated at initial metal concentrations of 0.5, 1.0 and 2.0 mM as competitive adsorbates using Arthrospira platensis and Chlorella vulgaris as biosorbents. The experimental results were evaluated in terms of equilibrium sorption capacity and metal removal efficiency and fitted to the multi-component Langmuir and Freundlich isotherms. The pseudo second order model of Ho and McKay described well the adsorption kinetics, and the FT-IR spectroscopy confirmed metal binding to both biomasses. Ni2+ and Zn2+ interference on Pb2+ sorption was lower than the contrary, likely due to biosorbent preference to Pb. In general, the higher the total initial metal concentration, the lower the adsorption capacity. The results of this study demonstrated that dry biomass of C. vulgaris behaved as better biosorbent than A. platensis and suggest its use as an effective alternative sorbent for metal removal from wastewater. (C) 2012 Elsevier B.V. All rights reserved.

Mimicking the pre-hairpin intermediate of gp41

A novel screening platform for potential retroviral fusion inhibitors on the basis of fully functional membrane‐anchored coiled coil lipopeptide receptors has been established. The work comprises the scrutiny of lateral organization of functional lipids in phase separated bilayers and an in‐depth investigation of the biophysical properties of lipopeptide‐based receptors. Lateral sorting of lipids was detected by the recognition of streptavidin of biotinylated lipids in phase separated bilayers and by nanoscopic patterns in mixed fluorocarbon / hydrocarbon lipid bilayers, employing temperature controlled atomic force microscopy (AFM) as a versatile characterization method. Particular features of fluorocarbon bilayers were additionally investigated in great detail by means of ellipsometry and ATR‐IR spectroscopy. Lipopeptide‐receptors were synthesized on the basis of a robust and reliable in situ coupling reaction by coupling terminal cysteine modified receptor‐peptides to a maleimide functionalized lipid bilayer. Receptor functionality of the lipopeptides was visualized by specific binding of vesicles and nanoparticles tracked by a multiplicity of characterization methods, such as AFM, ellipsometry, CLSM and fluorescence spectroscopy. Finally, in situ coupling of viral peptides, originating from the fusion protein of HIV resulted in a mimic of the pre‐hairpin intermediate of gp41. Structural analysis of N36‐lipopepides by means of CD‐spectroscopy in combination with FT‐IR spectroscopy revealed a coiled coil assembly of lipopeptides, which render the aggregates fully functional receptors for potent fusion inhibitors. Thereby, reversible inhibitor binding of T20 and the corresponding C‐ peptides was detected by AFM and ellipsometry, rendering coiled coil lipopeptides a new promising technique for screening of retroviral fusion inhibitors.

Herstellung hydrophiler Polyurethanpartikel und anisotroper Polymerpartikel

Hydrophile Polyurethanpartikel wurden mittels in inversen Miniemulsionen durchgeführten Polyadditionsreaktionen hergestellt. Wie durch FT-IR-Spektroskopie gezeigt wurde, konnte durch die Abwesenheit von Wasser in dem verwendeten System die Entstehung von Harnstoffbindungen vermieden werden. Das Molekulargewicht der erhaltenen Polyurethane konnte durch verschiedene Parameter, wie zum Beispiel die Hydrophobizität der kontinuierlichen Phase oder die Zugabe von DMSO zur dispersen Phase, beeinflusst werden. Die höchsten Molekulargewichte (Mn von bis zu 19000 g•mol-1) wurden mit Isopar M als kontinuierlicher Phase erhalten. Der zweite Teil der Arbeit beschäftigt sich mit der Herstellung anisotroper Polystyrolpartikel über eine Film-Dehnungs-Methode. Polystyrol/Polyvinylalkohol-Filme wurden oberhalb der Glasübergangstemperatur von Polystyrol und Polyvinylalkohol (Matrix) uniaxial oder biaxial gedehnt, wodurch ellipsenförmige oder scheibenförmige Partikel entstanden. Es zeigte sich, dass die Redispergierbarkeit der verstreckten Partikel in Wasser stark von deren Oberflächenfunktionalisierung abhängig war. Die beste Redispergierbarkeit (46%) wurde für Sulfonat-funktionalisierte Partikel erhalten. Als eine alternative Methode zur Herstellung anisotroper Polymerpartikel wurde im letzten Teil der vorliegenden Arbeit Elektrospinnen eingesetzt. Es konnte gezeigt werden, dass es prinzipiell möglich ist, ellipsenförmige PS-Partikel zu erhalten, deren Aspektverhältnis durch die Höhe der angelegten Spannung und den Abstand zwischen Spitze und Kollektor beeinflusst wurde. Neben PS-Partikeln konnten auch PMMA-Kapseln über Elektrospinnen verstreckt werden. Mittels der Film-Dehnungs-Methode konnte jedoch eine größere Vielfalt an Aspektverhältnissen hergestellt werden. Ein weiterer Nachteil gegenüber der Film-Dehnungs-Methode ist die relativ breite Größenverteilung der verstreckten Partikel. Jedoch ist Elektrospinnen im Gegensatz zur Film-Dehnungs-Methode ein kontinuierlicher Prozess und könnte auch für die Herstellung anisotroper Partikel von Polymeren mit einer hohen Glasübergangstemperatur verwendet werden.

PROPERTIES AND STRUCTURES OF Li-N BASED HYDROGEN STORAGE MATERIALS

Traditional transportation fuel, petroleum, is limited and nonrenewable, and it also causes pollutions. Hydrogen is considered one of the best alternative fuels for transportation. The key issue for using hydrogen as fuel for transportation is hydrogen storage. Lithium nitride (Li3N) is an important material which can be used for hydrogen storage. The decompositions of lithium amide (LiNH2) and lithium imide (Li2NH) are important steps for hydrogen storage in Li3N. The effect of anions (e.g. Cl-) on the decomposition of LiNH2 has never been studied. Li3N can react with LiBr to form lithium nitride bromide Li13N4Br which has been proposed as solid electrolyte for batteries. The decompositions of LiNH2 and Li2NH with and without promoter were investigated by using temperature programmed decomposition (TPD) and X-ray diffraction (XRD) techniques. It was found that the decomposition of LiNH2 produced Li2NH and NH3 via two steps: LiNH2 into a stable intermediate species (Li1.5NH1.5) and then into Li2NH. The decomposition of Li2NH produced Li, N2 and H2 via two steps: Li2NH into an intermediate species --- Li4NH and then into Li. The kinetic analysis of Li2NH decomposition showed that the activation energies are 533.6 kJ/mol for the first step and 754.2 kJ/mol for the second step. Furthermore, XRD demonstrated that the Li4NH, which was generated in the decomposition of Li2NH, formed a solid solution with Li2NH. In the solid solution, Li4NH possesses a similar cubic structure as Li2NH. The lattice parameter of the cubic Li4NH is 0.5033nm. The decompositions of LiNH2 and Li2NH can be promoted by chloride ion (Cl-). The introduction of Cl- into LiNH2 resulted in the generation of a new NH3 peak at low temperature of 250 °C besides the original NH3 peak at 330 °C in TPD profiles. Furthermore, Cl- can decrease the decomposition temperature of Li2NH by about 110 °C. The degradation of Li3N was systematically investigated with techniques of XRD, Fourier transform infrared (FT-IR) spectroscopy, and UV-visible spectroscopy. It was found that O2 could not affect Li3N at room temperature. However, H2O in air can cause the degradation of Li3N due to the reaction between H2O and Li3N to LiOH. The produced LiOH can further react with CO2 in air to Li2CO3 at room temperature. Furthermore, it was revealed that Alfa-Li3N is more stable in air than Beta-Li3N. The chemical stability of Li13N4Br in air has been investigated by XRD, TPD-MS, and UV-vis absorption as a function of time. The aging process finally leads to the degradation of the Li13N4Br into Li2CO3, lithium bromite (LiBrO2) and the release of gaseous NH3. The reaction order n = 2.43 is the best fitting for the Li13N4Br degradation in air reaction. Li13N4Br energy gap was calculated to be 2.61 eV.