983 resultados para Characterization physical chemistry
Resumo:
Objective. The purpose of this study was to evaluate the release of formaldehyde by some root canal filling materials. Study design. Two older endodontic sealers, AH 26 and Endomethasone, and 2 recently available sealers, AH Plus and Top Seal, were analyzed. Infrared and electronic spectroscopy were used to determine formaldehyde content after set of the materials. Results. Analysis showed that the AH 26 and Endomethasone sealers released formaldehyde. Although the AH Plus and Top Seal sealers have similar chemical composition, they released formaldehyde in a minimal concentration. Conclusions. The AH 26 and Endomethasone sealers released formaldehyde after setting; however, a minimum release was observed for the AH Plus and Top Seal sealers. Copyright © 1999 by Mosby, Inc.
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The formation of calcium silicate hydrates (C-S-H) during the hydration of tricalcium silicate (C3S) in pure water and in water solutions containing 1% CaCl2 (accelerator) and 0.01% saccharose (retarder) was studied by small-angle X-ray scattering (SAXS). SAXS measurements were performed under isothermal conditions within the temperature range 25 °C T < 52 °C. The experimental results indicate that the time variation of the mass fraction of the C-S-H product phase, α(f), can be fitted, under all conditions of paste setting, by Avrami equation, α(t) = 1 -exp(-(kt)′), k being a rate parameter and n an exponent depending on the characteristics of the transformation. The parameter n is approximately equal to 2 for hydration of C^S in pure water. Depending on temperature, n varies from 2 to 2.65 for hydration in the presence of CaC^ and saccharose. The value n = 2 is theoretically expected for lateral growth of thin C-S-H plates of constant thickness. The time dependence of SAXS intensity indicates that the transformed phase (C-S-H) consists of colloidal particles in early stages of hydration, evolving by two-dimensional growth toward a disordered lamellar structure composed of very thin plates. The activation energy ΔE for the growth of C-S-H phase was determined from the time dependence of X-ray scattering intensity. These data were obtained by in situ measurements at different temperatures of hydration. The values of ΔE are 37.7, 49.4, and 44.3 kJ/mol for hydration in pure water and in water solutions containing CaCl2 and saccharose, respectively. © 2000 American Chemical Society.
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The conformational transition from coil to extended coil for polygalacturonic acid has been studied by conductometric titrations and Monte Carlo simulations. The results of conductometric titrations at different polymer concentrations have been analyzed using the model proposed by Manning,1 which describes the conductivity of polyelectrolitic solutions. This experimental approach provides the transport factor and the average distance between charged groups at different degrees of ionization (α). The mean distances between charged groups have been compared with the values obtained by Monte Carlo simulations. In these simulations the polymer chain is modeled as a self-avoiding random walk in a cubic lattice. The monomers interact through the unscreened Coulombic potential. The ratio between the end-to-end distance and the number of ionized beads provides the average distance between charged monomers. The experimental and theoretical values are in good agreement for the whole range of ionization degrees accessed by conductometric titrations. These results suggest that the electrostatic interactions seem to be the major contribution for the coil to extended coil conformational change. The small deviations for α ≤ 0.5 suggests that the stiffness of the chain, associated with local interactions, becomes increasingly significant as the fraction of charged groups is decreased. © 2000 American Chemical Society.
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Infrared and photoluminescence spectroscopies have been used to investigate the local environment of the Eu3+ ions in luminescent sol-gel derived materials-di-ureasils-based on a hybrid framework represented by U(600). This host is composed of a siliceous backbone grafted, through urea cross-links, to both ends of polymer segments incorporating 8.5 oxyethylene repeat units. The active centers have been introduced as europium perchlorate, Eu(ClO4)3. Samples with compositions n = 232, 62, 23, 12, and 6 (where n denotes the ratio of (OCH2CH2) moieties per lanthanide ion) have been examined. The combination of the information retrieved from the analysis of characteristic bands of the FTIR spectra-the perchlorate and the Amide I/Amide II features-with that obtained from the photoluminescence data demonstrates that at compositions n = 232 and 62 the anions are free, whereas the Eu3+ ions are complexed by the heteroatoms of the polyether chains. At higher salt concentration, the cations are bonded, not only to the ClO4 - ions, but also to the ether oxygen atoms of the organic segments and to the carbonyl oxygen atoms of the urea linkages. The dual behavior of U(600) with respect to cation coordination has been attributed to the presence in this nanohybrid of strong hydrogen-bonded urea-urea structures, which, at low salt content, cannot be disrupted, thus inhibiting the formation of Eu3+-O=C(urea) contacts and promoting the interaction between the lanthanide ions and the (OCH2CH2) moieties. The present work substantiates the claim that the activation of the coordinating sites of the di-ureasil framework can be tuned by varying either the guest salt concentration at constant chain length or the length of the.organic segments at constant salt concentration. This relevant property opens challenging new prospects in the fields of application of this class of hybrids. © 2001 American Chemical Society.
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Aim: To evaluate the release of calcium ions, pH and conductivity of a new experimental dental cement (EC) and to compare them with those of mineral trioxide aggregate (MTA-Angelus). Methodology: Five samples of each cement were prepared using plastic tubes 1 mm in diameter and 10 mm long. Each sample was sealed in a test tube containing 10 mL deionized water which was analysed after 24, 48, 72, 96, 192, 240 and 360 h for pH, electrical conductivity and calcium release. The concentration of calcium ions was obtained through atomic absorption spectroscopy technique. The data were analysed statistically using the analysis of variance (ANOVA) and the Student's test (t-test). Results: The pH of the storage solutions was not affected by the material and the interaction of material with time (P > 0.05). However, the time of immersion was significant (P < 0.01) for both materials. For the electric conductivity and calcium release, the interaction of material with time was statistically significant (P < 0.01), indicating that EC and MTA-Angelus did not behave in a similar manner. Conclusions: The experimental cement released calcium and increased the pH of the storage solutions in a similar manner to MTA-Angelus. However, EC showed significantly higher calcium release than commercial MTA-Angelus after 24 h. © 2005 International Endodontic Journal.
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The (Sn,Ti)O2, system has a great interest due to its technological applications such as gas sensor and varistor. Although the thermodynamic properties and the kinetics of spinoidal decomposition in this system have been extensively studied, the general properties and applications of SnO2 - TiO2 binary compositions have been not investigated yet in depth. On the other hand, little work has been done to optimize the synthesis methods to obtain (Sn,Ti)O2 cerallmic powders, with pre - determinate physical and chemical characteristics. In this work the ceramic powders has been obtained by coprecipitation and polymeric precursor (Pechini) methods. The different physical chemistry phenomena that occurred during the synthesis were discussed. The (Sn,Ti)O2, ceramic powders were characterized with X- ray diffraction (XRD), thermal analysis (DTA/TG) and scanning electron microscopy (SEM). The knowledge about of steps and variables of synthesis process acquired with development of this work, we permited to obtain (Sn, Ti)O2, nanometers particles to low temperatures: to 450°C for coprecipitation method and to 600°C for Pechini method. The spinodal decomposition that ocurr to 900°C was discussed also.
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In this work, a micellar system of benzathine penicillin G (BPG) in sodium deoxycholate (NaDC) was developed and evaluated physicochemically. The solubility profile of the drug in water and buffer solutions at various pH was determined, as well as its n-octanol/water partition coefficient. The Critical Micellar Concentration of NaDC and its ability to incorporate BPG were also assessed. The study was carried out at low and high ionic strength which was adjusted by the addition of sodium chloride. The results demonstrated the ability of the micellar system to incorporate BPG, as well as to increase its apparent solubility in water. The enhancement of the solubility of BPG by the presence of NaDC micelles could be analyzed quantitatively within the framework of the pseudo-phase model. Concentration analysis showed that the micellar system could attain up to 90% incorporation of BPG. The incorporated drug is expected to exhibit improved stability, since the antibiotic enclosed in the hydrophobic core of micelles is rather shielded from the aqueous external environment.
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Aqueous dispersions of monoolein (MO) with a commercial hydrophobically modified ethyl hydroxyethyl cellulose ether (HMEHEC) have been investigated with respect to the morphologies of the liquid crystalline nanoparticles. Only very low proportions of HMEHEC are accepted in the cubic and lamellar phases of the monoolein-water system. Due to the broad variation of composition and size of the commercial polymer, no other single-phase regions were found in the quasi-ternary system. Interactions of MO with different fractions of the HMEHEC sample induced the formation of lamellar and reversed hexagonal phases, identified from SAXD, polarization microscopy, and cryogenic TEM examinations. In excess water (more than 90 wt %) coarse dispersions are formed more or less spontaneously, containing particles of cubic phase from a size visible by the naked eye to small particles observed by cryoTEM. At high polymer/MO ratios, vesicles were frequently observed, often oligo-lamellar with inter-lamellar connections. After homogenization of the coarse dispersions in a microfluidizer, the large particles disappeared, apparently replaced by smaller cubic particles, often with vesicular attachments on the surfaces, and by vesicles or vesicular particles with a disordered interior. At the largest polymer contents no proper cubic particles were found directly after homogenization but mainly single-walled defected vesicles with a peculiar edgy appearance. During storage for 2 weeks, the dispersed particles changed toward more well-shaped cubic particles, even in dispersions with the highest polymer contents. In some of the samples with low polymer/MO ratio, dispersed particles of the reversed hexagonal type were found. A few of the homogenized samples were freeze-dried and rehydrated. Particles of essentially the same types, but with a less well-developed cubic character, were found after this treatment. © 2007 American Chemical Society.
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This study evaluated the water quality of the Vargem Limpa stream and tested the hypothesis that protected stretches of the aquatic system, located within a conservation unit, favor the preservation of the diversity of Chironomidae (Insecta: Diptera). Samplings were conducted in four stations, where some physical and chemical variables were measured. The results obtained by the study indicated the predominance of genera associated with arenaceous substrata, and that the stretches protected by the conservation unit presented better environmental conditions, with better-preserved Chironomidae diversity, demonstrating the importance of these areas in maintaining the diversity of Chironomidae.
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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.
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Considering the quality of the phytotherapic agents, it is important to point out that it includes rigorous attendance of the different steps of the development and production of these products, from the collection of the vegetable to the availability of the final product. In this work the quality control of the Operculina macrocarpa (Linn) Urb. roots, popularly known as 'batata-de-purga', was carried out. Pharmacopoeic and no pharmacopoeic methodologies were employed to physico-chemical and microbiological quality control. The obtained results showed that the roots presents a content of resin of 9,85%, The microbiological analysis did not present pathogenic growth among the other accomplished tests. The work stands out the importance of the establishment of norms for the quality control for the plants, so that they are found able to be used for phytotherapic reasons.
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This study describes the chemical and physical-chemical profile of plant drug and ethanolic extract obtained from fruits of Solanum lycocarpum A. St.-Hill. (Solanaceae). The physical and chemical analysis involved the granulometry determination, non-compacted apparent density, loss on drying in oven and in infrared scale, pH, ash values and extractive values. The results determined the physical-chemical characteristics of the drug plant. It was also carried out the microbiological control of the plant drug. The preliminary phytochemical screening featured the presence of tannins, flavonoids and saponins in the plant drug and alkaloids and steroids in the ethanolic exctract. The solamargine and solasonine glycoalkaloids were identified through TLC and GC/ MS. The levels of total phenols and tannins were quantified in the extract (8.90% and 6,85% respectively). Such studies contribute to the chemical identification and quality control of S. lycocarpum fruits. © 2010 Phcog.net.
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Praziquantel (PZQ) is the drug of choice commonly used for the treatment of shistosomiasis. However, it has low aqueous solubility, which could limit its bioavailability in the body. To circumvent these features, an inclusion complex with hydroxypropyl-beta- cyclodextrin (HP-β-CD) was prepared. Thus, the objective of this work was to prepare and characterize the PZQ/HP-β-CD inclusion complex. Morphological, spectroscopic, and calorimetric analysis showed the first signs of the guest/host interaction. The complexation kinetic analysis was used to determine the kinetic constant and, besides that, it was possible to establish the time consumed to reach equilibrium. Using the solubility isotherm, it was observed that the interaction with HP-β-CD increased 2.4 fold the aqueous solubility of plain PZQ. In vitro cytotoxicity tests, using fibroblast cells, evidenced no toxicity for these cells at the concentrations tested. These results demonstrated that there is a potential use of PZQ in formulations with HP-β-CD.