Thermogravimetric data were used to calculate the kinetics of isothermal degradation of layered tetratitanate intercalated
with n-alkyldiamines H2N(CH2)nNH2 (n=2, 3, 4, 6 or 8). The hydrous matrix showed two mass loss steps from the thermogravimetric curve, corresponding to the release
of physisorbed and lattice water molecules. For the intercalated matrices a third mass loss was observed due to the release
of organic moiety. From these values, the amine intercalated matrices can be ordered in the following sequence of thermal
stability; C4>C2>C3≅C6>C8. Kinetic studies were carried out to the release of lattice water molecules. The kinetic model that
best adjusted the experimental isothermal TG data was the diffusion mechanism controlling process.
Authors:J. Mano, S. Lanceros-Méndez, A. Nunes and M. Dionísio
Dielectric experiments are often performed in non-isothermal conditions. Thus, there is a difference between the temperature of the sample and the sensor temperature. In this work we propose and compare three temperature calibration methods based on the detection of transitions or relaxations: i) the melting of high-purity metallic standards (indium and tin), ii) the 2nd order phase transition of a ferroelectric crystal (TGS); iii) the -relaxation of an amorphous polymer (poly(carbonate)). The results obtained from the three different methods were used to construct a calibration curve for a given heating rate.
Authors:M. Brito, Gabriela Barin, A. Araújo, D. de Sousa, S. Cavalcanti, Ana Lira and Rogéria Nunes
The aim of this work was to study the effect of Lippia sidoides essential oil (LSEO) on stratum corneum lipids and the permeation of salicylic acid. DSC and FTIR spectroscopy were applied.
LSEO 1% (v/v) significantly enhanced salicylic acid flux through snake skin. According to the DSC curves changes in the transition
temperature of the lipids were observed indicating that LSEO can interact with stratum corneum. The IR spectrum of skin treated
with LSEO showed a decrease in the peak intensity for CH2 stretchings (2920–2850 cm–1) however the peak positions did not alter suggesting the extraction of the lipids.
Authors:A. Souza, M. Oliveira, I. Santos, M. Conceição, L. Nunes and J. Machado
The kinetics of thermal decomposition of solid In(S2CNR2)3 complexes, (R=CH3, C2H5, n-C3H7,i-C3H7, n-C4H9 and i-C4H9), has been studied using isothermal and non-isothermal thermogravimetry. Superimposed TG/DTG/DSC curves show that thermal
decomposition reactions occur in the liquid phase, except for the In(S2CNMe2)3 and In(S2CNPri2)3 compounds.
Authors:J. Botelho, A. Souza, L. Nunes, A. Chagas, I. Garcia dos Santos, M. da Conceição and P. Dunstan
The standard molar enthalpies of formation of crystalline dialkyldithiocarbamates chelates, [Pd(S2CNR2)2], with R=C2H5, n-C3H7, n-C4H9 and i-C4H9, were determined through reaction-solution calorimetry in acetone, at 298.15 K. From the standard molar enthalpies of formation
of the gaseous chelates, the homolytic (172.43.8, 182.53.2,150.93.1 and 162.63.1 kJ mol−1) and heterolytic (745.03.8, 803.73.3,834.33.1 and 735.23.0 kJ mol−1) mean palladium-sulphur bond-dissociation enthalpies were calculated.
Authors:Paula Nunes, Marília Bezerra, L. Costa, Juliana Cardoso, R. Albuquerque, M. Rodrigues, Gabriela Barin, Francilene da Silva and A. Araújo
The purpose of this study was to evaluate the physical–chemical properties of collagen (CL) and usnic acid/collagen-based
(UAC) films, using differential thermal analysis (DTA), thermogravimetry (TG/DTG), infrared spectroscopy (FTIR), and scanning
electron microscopy (SEM). Both films were prepared by casting process using polyethylene glycol 1500 (PEG 1500) as plasticizer.
In the spectrum of UAC, similar bands of the usnic acid are observed, indicating that the polymerization (film formation)
did not affect the stability of the drug. Distinctly, DTA curve of UAC did not show an endothermic peak at 201 °C, indicative
that the drug was incorporated into the polymeric system. These results were corroborated by the scanning electron microscopy
(SEM). The TG/DTG curves of UAC presented a different thermal decomposition profile compared to the individual compounds and
CL. These findings suggest the occurrence of molecular dispersion or solubilization of the drug in the collagen film.
Authors:J. R. Azevedo, R. H. Sizilio, M. B. Brito, A. M. B. Costa, M. R. Serafini, A. A. S. Araújo, M. R. V. Santos, A. A. M. Lira and R. S. Nunes
The purpose of this study was to develop and characterize insulin nanoparticles systems using chitosan. Insulin-loaded nanoparticles were prepared by ionic gelation of chitosan with tripolyphosphate anions (TPP). The interactions between insulin and chitosan were evaluated by differential scanning calorimetry (DSC), thermogravimetry/derivative thermogravimetry (TG/DTG), and Fourier-transform infrared (FTIR) spectroscopy. Besides, particle size distribution, polydispersity index (PDI), zeta potential, and association efficiency (AE%) of the nanoparticles were evaluated. In general, inert nanoparticles and insulin-loaded nanoparticles showed an average size of 260.56 nm (PDI 0.502) and 312.80 nm (PDI 0.481), respectively. Both nanoparticles showed positive charge, but after insulin incorporation the zeta potential was reduced, evidencing its incorporation. Nanoparticles obtained also showed AE% around 70%, measured by high-performance liquid chromatography (HPLC). The results of FTIR, DSC, and TG/DTG corroborated the data presented suggesting that insulin was successfully encapsulated. However, drug incorporation seems to be related not only to electrostatic interactions, but also to physical process and/or adsorption phenomena.
Authors:Ellen Denise P. Almeida, Adjane A. Costa, Mairim R. Serafini, Fábia C. Rossetti, Juliana M. Marchetti, Victor Hugo V. Sarmento, Rogéria de S. Nunes, Mário Ernesto G. Valerio, Adriano A.S. Araújo and Ana Amélia M. Lira
Solid lipid nanoparticles (SLN) without drug and SLN loaded with chloroaluminum phthalocyanine (AlClPc) were prepared by solvent diffusion method in aqueous system and characterized by thermal analyses and X-ray diffraction (XRD) in this study. Determination of particle size, zeta potential (ZP), and encapsulation efficiency were also evaluated. SLN containing AlClPc of nanometer size with high encapsulation efficiency and ZP were obtained. The results indicated that the size of SLN loaded with AlClPc is larger than that of the inert particle, but ZP is not changed significantly with incorporation of the drug. In differential scanning calorimetry (DSC) curves, it was observed that the melting point of stearic acid (SA) isolated and in SLN occurred at 55 and 64 °C, respectively, suggesting the presence of different polymorphs. DSC also shows that the crystallinity state of SLN was much less than that of SA isolated. The incorporation of drug in SLN may have been favored by this lower crystallinity degree of the samples. XRD techniques corroborated with the thermal analytic techniques, suggesting the polymorphic modifications of stearic acid.