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  • Author or Editor: M. Arias x
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Abstract  

The evaporation of octanoic (caprylic) acid was investigated by means of thermogravimetric analysis (temperature range: 300–600 K) under a nitrogen dynamic atmosphere (heating rates: 0.16, 0.31, 0.63, 1.25, 2.5, 5 and 10 K min−1). Kinetic plots for a zero-order process were constructed based on the Arrhenius equation. The activation energy for the evaporation process was calculated via both the Arrhenius plot and Vyazovkin’s isoconversional model-free method.

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Abstract  

This paper examines binary polyethyleneglycol (molecular weight 6000)-Triamterene (PEG 6000-T) solid dispersions (5–40 w/w% of T) prepared by the fusion carrier method, and physical mixtures (5–90 w/w% of T) are studied using DSC and Hot Stage Microscopy (HSM). The use of these combined techniques allows to explain the thermal behaviour on the basis of dissolution of T in the liquid carrier according to the progressive disappearance of the original crystals over a wide range of temperatures (ca. 100°C). The above fact, and possibly the sublimation of T, also could explain that at low T content (<- 30 w/w%), DSC curves exhibited only a single endothermic peak and/or weak endothermic peaks. On the basis of DSC data, a tentative phase diagram of this system is proposed.

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Abstract  

Thermal analysis (DSC and HSM), and equilibrium solubility determinations were carried out to elucidate the mechanism of interaction at the solid state in the binary system triamterene-D-mannitol. Physical mixtures (5–90% w/w triamterene) and solid dispersions (5 up to 40% w/w triamterene) were prepared and studied. From DSC and HSM results, the thermal changes were associated with the variations in composition of the binary mixture, being more pronounced in the range 20–50% w/w. The binary phase diagram was proposed, although the exact position of the eutectic was uncertain. This is in accordance with a partial dissolution process detected by HSM. A linear increase in the solubility of triamterene with increasing aqueous mannitol concentration was obtained. The thermodynamic parameters of the solution properties were calculated, with an activation energy value of 96.081 kJ/mole. The solubilization increase was associated with complexation processes and hydrogen bonding formation.

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Journal of Thermal Analysis and Calorimetry
Authors: P. Sánchez-Soto, M. Villacampa, J. Ginés, A. Ruiz-Conde, M. Avilés and M. Arias

Abstract  

Several derivatives containing a new organic ring system, the tropane-6-spiro-5′-hydantoin structure (namely 8-alkyl-8-azabicyclo [3.2.1.] octane-6-spiro-5′-imidazoline-2′,4′-diones) have been characterized by thermal (DSC and simultaneous DTA-TG-DTG) and spectroscopic techniques (IR,1 H-NMR,13 C-NMR). X-ray powder diffraction and elemental analysis were applied for structural and molecular characterization. All the compounds melt in the range 160–250°C and undergo decomposition with progressive mass loss after the solid-liquid thermal transition with molecular degradation. It was found that tropane-6-spiro-5′-hydantoin derivatives with the hydantoin ring in β position are thermally less stable than those containing this ring in α position.

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The effectiveness of five commercial disinfectants used in the food industry was evaluated against different strains isolated from foodborne outbreaks (E. coli O157:H7, Salmonella spp. and L. monocytogenes) and a collection strain (S. aureus) in an aqueous suspension medium. The disinfectants evaluated included quaternary ammonium compounds, aldehydes, hydrogen peroxide and peracetic acid, clorhexidine and a tertiary alkylamine.  In the absence of organic matter, all the disinfectants tested were effective with an exposure time of 10 min at the lowest concentration recommended by the manufacturer. However, in the presence of organic matter their effectiveness decreased. The most effective disinfectant against pathogenic bacteria tested was a quaternary ammonium compound based disinfectant combined with non-ionic surfactants, polyphosphates and alkaline salts. The least effective ones were disinfectants containing tertiary alkylamine, peracetic acid and hydrogen peroxide.

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Abstract

Microcalorimetry is an experimental technique which allows us to precisely measure the energy released as a consequence of any transformation process. All organisms produce heat as a consequence of metabolism. The rate of heat production is an adequate measurement of metabolic activity of organisms and their constituent parts, cells and sub-cellular levels. Microorganisms produce small amounts of heat, in the order of 1–3 pW per cell. Despite the low quantity of heat produced by bacteria, their exponential replication in culture medium allows their detection using microcalorimetry. This study is a microcalorimetric study of the growth and metabolism of the bacterium Pseudomonas aeruginosa, using the heat liberated as a consequence of bacterial metabolism. With this aim, we used a Calvet microcalorimeter, inside which two Teflon screw-capped stainless steel cells were located (sample and reference). Experiments were carried out at final concentrations of 106, 105, 103 and 10 CFU/mL, and a constant temperature of 309.65 K was maintained within the microcalorimeter. Recording the difference in calorific potential over time we obtained P. aeruginosa’s growth curves. The shape of these curves is characteristic and has a single phase. Thus, the heat flow curves were mathematically studied to calculate the growth constant and generation time of this bacterium.

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Journal of Radioanalytical and Nuclear Chemistry
Authors: A. Arias, A. Arias, M. Oddone, M. Oddone, G. Bigazzi, G. Bigazzi, A. Di Muro, A. Di Muro, C. Principe, C. Principe, P. Norelli and P. Norelli

Summary  

Newly produced fission track (FT), instrumental neutron activation analysis (INAA) and micro-Raman spectrometry data have been used to characterize the classical source areas of the Milos obsidians better and to check the provenance of obsidian artefacts. The Bombarda-Adhamas and Demenegaki obsidians yielded indistinguishable FT ages 1.57±0.12 and 1.60±0.06 My, respectively, in agreement with previous FT data. By INAA analyses it was possible to discriminate between the three obsidian sources on Milos: Bombarda-Adhamas, Demenegaki and A. Ioannes. Raman spectroscopy has been found to be a valuable technique to gain a chemico-structural characterization of a given obsidian population in terms of dissolved water content and microlite distribution/composition.

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Abstract

Enterococcus faecalis is a Gram-positive bacteria, considered one of the most common causes of nosocomial infections. Bacterial cultures produce an exchange of energy as a result of the bacteria metabolisms. The rate of heat production is an adequate measure of the metabolic activity of the organisms and their constituent parts. Microorganisms produce small amounts of heat: 1–3 pW per cell. Although the heat produced by bacteria is very small, their exponential reproduction in a culture medium permits heat detection through microcalorimetry. In this study, we analyzed the microcalorimetric behavior of Enterococcus faecalis. A thermal Calvet microcalorimeter was used. The inside of the calorimeter contains two stainless steel cells (experimental and reference). Experiments were carried out at final concentrations of 106,105,103, and 10 CFU/mL and a constant temperature of 309.65 K was maintained within the microcalorimeter. Recording the difference in calorific potential over time we obtained E. faecalis’s growth curves. Thermograms were analyzed mathematically allowing us to calculate the constant growth, generation time and the amount of heat exchanged over the culture time.

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Journal of Thermal Analysis and Calorimetry
Authors: O. Ayala, D. Lardizábal, A. Reyes, M. Rosales, J. Matutes and A. González Arias

Abstract  

Expressions for calculating the cation vacancy contents of MnZn ferrites from thermogravimetric curves are presented together with some experimental data. In a single-phase MnZn ferrite synthesized by conventional ceramic procedures, the O2 evolution accompanying ferrite formation follows the formal equation. Mn2+ σα Znσβ Fe3+ 2σ(1–γ) [V ]σ/4(1–2γ) O4 =σ'/σ Mn2+ σ(α–2ϕ) Znσβ Fe2+ 2σθ Mn3+ 2σϕ Fe3+ 2σ(1–γ–θ) [V ]σ/4(1–2γ–3ϕ) O4 +σ'φ/2O2 (g) where α and β denote the MnO and ZnO mole fractions in the primary mixture γ=α+β, θ and ϕ depend on the quantities of Fe2+ and Mn3+ formed, respectively, φ=θ–ϕ and σ'/σ is a function of the former parameters. Even though the relative amounts of Fe2+ /Fe3+ and Mn2+ /Mn3+ remain uncertain, the vacancy content [V ] of the ferrite can be determined because it depends on φ alone, which is related to the change in mass of the sample as the synthesis takes place through the equation φ=(1.5–γ) µβO2 (1–m f /m i ) Here, m i and m f are the masses of the sample before and after O2 evolution, µB is the formula mass of the ferrite and µO2 is the O2 molar mass. Practically vacancy-free single-phase MnZn ferrite samples were obtained by sintering in air at 1250°C and cooling in pure N2 .

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Abstract  

In this work a series of solid sorbents were synthesized by immobilizing liquid amines on the surface of a mesoporous alumina. The samples were chemically characterized and BET surface areas calculated from the N2 adsorption isotherms at 77 K. The CO2 capture performance of the sorbents and their thermal stability was studied by thermogravimetric methods. The effect of amine loading on the CO2 capture performance of the prepared sorbents was also evaluated. Analysis of TG-DTG curves showed that thermal stabilization of the amines is significantly improved by immobilizing them on an inorganic support. Temperature-programmed CO2 adsorption tests from 298 K up to 373 K at atmospheric pressure, proved to be a useful technique for assessing the capacity of sorbents for CO2 capture. Alumina impregnated with diethylenetriamine presented the highest CO2 adsorption capacities throughout the tested temperature range.

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