Synthesis, characterization and thermal behaviour of solid-state compounds of light trivalent lanthanide succinates

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

Thermal and spectroscopic data to investigate the oxamic acid, sodium oxamate and its compounds with some bivalent transition metal ions

Synthesis, characterization, and thermal behavior of transition metal oxamates, M(NH(2)C(2)O(3))(2)center dot nH(2)O (M = Mn(II), Fe(II), Co(II), Ni(II), Cu(II), Zn(II)), as well as the thermal behavior of oxamic acid and its sodium salt (NaNH(2)C(2)O(3)) were investigated employing simultaneous thermogravimetry and differential scanning calorimetry (TG-DSC), experimental and theoretical infrared spectroscopy, TG-DSC coupled to FTIR, elemental analysis and complexometry. The results led to information about the composition, dehydration, thermal stability, thermal decomposition, as well as of the gaseous products evolved during the thermal decomposition of these compounds in dynamic air and N(2) atmospheres.

Thermal behaviour of succinic acid, sodium succinate and its compounds with some bivalent transition metal ions

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

Synthesis, characterization and thermal behaviour of heavy lanthanide and yttrium pyruvates in the solid state

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

Two thermal methods to measure the energy fluence of a brief exposure of diagnostic x rays

This paper describes two simple thermal methods for measuring the energy fluence in J/cm 2 from a diagnostic x-ray exposure. Both detectors absorb essentially 100% of the radiation and give a signal that is directly proportional to the energy fluence of the x-ray beam. One detector measures the thermal effect when a pulse of x rays is totally absorbed in the pyroelectric detector of lead-zirconium-titanate (PZT). The other detector measures the expansion of a gas surrounding a lead disk detector in a photoacoustic chamber. The increased pressure of the gas is transmitted through a 1-mm duct to a sensitive microphone. Both detectors have previously been used to measure the energy fluence rate of continuous x-ray beams in the same energy region using a chopped beam and a lock-in amplifier. Measurement of the energy fluence of a pulse of radiation eliminates the need for the beam chopper and lock-in amplifier and results in a simple, rugged, and inexpensive dosimeter. Either method can be combined with the area of the beam to give an estimate of the imparted energy to the patient from a diagnostic x-ray exposure.

PCM thermal insulation in buildings

This paper presents the results of a numerical and experimental study of phase change material (PCM) filled walls and roofs under real operational conditions to achieve passive thermal comfort. The numerical part of the study was based on a one-dimensional model for the phase change problem controlled by pure conduction. Real radiation data was used to determine the external face temperature. The numerical treatment was based upon using finite difference approximations and the ADI scheme. The results obtained were compared with field measurements. The experimental set-up consisted of a small room with movable roof and side wall. The roof was constructed in the traditional way but with the phase change material enclosed. Thermocouples were distributed across the cross section of the roof. Another roof, identical but without the PCM, was also used during comparative tests. The movable wall was also constructed as is done traditionally but with the PCM enclosed. Again, thermocouples were distributed across the wall thickness to enable measurement of the local temperatures. Another wall, identical but without the PCM, was also used during comparative tests. The PCM used in the numerical and experimental tests was composed of a mixture of two commercial grades of glycol in order to obtain the required fusion temperature range. Comparison between the simulation results and the experiments indicated good agreement. Field tests also indicated that the PCM used was adequate and that the concept was effective in maintaining the indoor temperature very close to the established comfort limits. Further economical analysis indicated that the concept could effectively help in reducing the electric energy consumption and improving the energy demand pattern. © 1997 by John Wiley & Sons, Ltd.

Control of thermal damage in grinding by digital signal processing of raw acoustic emission

Grinding process is usually the last finishing process of a precision component in the manufacturing industries. This process is utilized for manufacturing parts of different materials, so it demands results such as low roughness, dimensional and shape error control, optimum tool-life, with minimum cost and time. Damages on the parts are very expensive since the previous processes and the grinding itself are useless when the part is damaged in this stage. This work aims to investigate the efficiency of digital signal processing tools of acoustic emission signals in order to detect thermal damages in grinding process. To accomplish such a goal, an experimental work was carried out for 15 runs in a surface grinding machine operating with an aluminum oxide grinding wheel and ABNT 1045 e VC131 steels. The acoustic emission signals were acquired from a fixed sensor placed on the workpiece holder. A high sampling rate acquisition system at 2.5 MHz was used to collect the raw acoustic emission instead of root mean square value usually employed. In each test AE data was analyzed off-line, with results compared to inspection of each workpiece for burn and other metallurgical anomaly. A number of statistical signal processing tools have been evaluated.

Temperature analysis during bonding of brackets using LED or halogen light base units

The purpose of our investigation is to compare the intrapulpal temperature changes following blue LED system and halogen lamp irradiation at the enamel surface of permanent teeth. The fixation of brackets using composite resin is more comfortable and faster when using a photo-curable composite. Several light sources can be used: halogens, arc plasma, lasers, and recently blue LED systems. An important aspect to be observed during such a procedures is the temperature change. In this study, we have used nine human extracted permanent teeth: three central incisors, three lateral incisors, and three canines. Teeth were exposed to two light sources: blue LED system (preliminary commercial model LEC 470-II) and halogen lamp (conventional photo-cure equipment). The surface of teeth was exposed for 20, 40, and 60 sec at the buccal and lingual enamel surface with an angle of 45 degrees. Temperature values measured by a thermistor placed at pulpar chamber were read in time intervals of 1 sec. We obtained plots showing the temperature evolution as a function of time for each experiment. There is a correlation between heating quantity and exposition time of light source: with increasing exposition time, heating increases into the pulpal chamber. The halogen lamp showed higher heating than the LED system, which showed a shorter time of cooling than halogen lamp. The blue LED system seems like the indicated light source for photo-cure of composite resin during the bonding of brackets. The fixation of brackets using composite resin is more comfortable and faster when using a photo-curable composite. Blue LED equipment did not heat during its use. This could permit a shorter clinical time of operation and better performance. © Mary Ann Liebert, Inc.

Synthesis, characterization and thermal behaviour of solid-state compounds of 4-methoxybenzoate with some bivalent transition metal ions

Solid-state M-4-MeO-Bz compounds, where M stands for bivalent Mn, Co, Ni, Cu and Zn and 4-MeO-Bz is 4-methoxybenzoate, have been synthesized. Simultaneous thermogravimetry-differential thermal analysis (TG-DTA), differential scanning calorimetry (DSC), X-ray powder diffractometry, infrared spectroscopy, elemental analysis and complexometry were used to characterize and to study the thermal behaviour of these compounds. The results led to have information about the composition, dehydration, thermal stability and thermal decomposition of the isolated compounds. © 2005 Akadémiai Kiadó, Budapest.

Heating rate and temperature effects on the BaTiO3 formation by thermal decomposition of (Ba,Ti) organic precursors during the Pechini process

Different thermal treatments for the synthesis of BaTiO3 powder obtained through the Pechini method were studied. The synthesis of BaTiO3 starts at 150 °C by the thermal dehydration of organic precursors. The usual inevitable formation of barium carbonate during the thermal decomposition of the precursor could be retarded at lower calcination temperatures and optimized heating rates. The organic precursors were treated at temperatures between 200 and 400 °C. Then, the samples were calcined at 700 and 800 °C for 4 and 2 h, respectively. The resulting ceramic powders were characterized by gravimetric and differential thermal analyses, X-ray powder diffraction and infrared spectroscopy. It was found that depending on the heating rate and final temperature of the thermal treatment, high amounts of BaCO3 and TiO2 could be present due to the high concentration of organics in the final calcination step. © 2007 Elsevier B.V. All rights reserved.

Blood parameters of chicks from eggs injected with ascorbic acid and subjected to thermal stress

This study was aimed to verify if chicks from eggs injected with ascorbic acid and subjected to thermal stress would have higher immunity than chicks from incubation at thermoneutrality without injection of ascorbic acid. The parameters evaluated were temperature on oxygen saturation in hemoglobin, glucose, number of erythrocytes, hematocrit rate and number of hemoglobins of newly hatched male chicks, hatched from eggs injected with ascorbic acid (AA) and subjected to thermal stress during incubation. The experimental design was completely randomized in factorial scheme 5 (application levels of ascorbic acid) x 2 (incubation temperatures). The data were subjected to analysis of variance using the General Linear Model procedure (GLM) of SAS ®. For the parameters (number of erythrocytes, rate of hematrocit and values of hemoglobin), there was significant interaction (p <0.05) between treatments in egg and incubation temperatures. Analyzing the interactions for these parameters, it was observed that the application of 0% ascorbic acid in egg minimized the effect of heat stress when compared with treatment without injection. The application of ascorbic acid levels in eggs incubated under heat stress failed to maximize the immunity of newly hatched chicks. It is assumed that the increased liquid in the amniotic fluid, in those embryos injected with water, favored the lower heat conductance for these embryos, thus helping in their development in relation to immunity. Considering that hemoglobin is related to the transport of gases, these data suggest that increasing the concentration of AA solution inoculated may influence the respiratory rates of eggs.

Balance of pH of chicks from eggs injected with ascorbic acid and subjected to thermal stress

This study aimed to verify that chicks from eggs injected with ascorbic acid and subjected to heat stress would have changes in acid-base balance, compared to chicks incubated at thermoneutral without injection of ascorbic acid. The parameters evaluated were blood pressure of carbon dioxide and oxygen, base excess, total carbon dioxide, concentration of sodium, potassium, ionized calcium, bicarbonate and pH of newly hatched male chicks, hatched from eggs injected with acid ascorbic acid (AA) and subjected to heat stress during incubation. The experimental design was completely randomized in factorial scheme 5 (application levels of ascorbic acid) x 2 (incubation temperatures). The data were subjected to analysis of variance using the General Linear Model procedure (GLM) of SAS ®. For the blood pH was observed significant interaction (p <0.05) between treatments with application in eggs and incubation temperatures. For the other parameters were not significant effects (p< 0.05) of AA level and neither temperature of incubation. Analyzing the unfolding of the interaction to pH was observed that chicks from eggs injected with 6% ascorbic acid and subjected to heat stress during incubation had a higher pH value compared with the thermoneutral temperature incubated (p <0.05). Therefore, it is suggested that the incubation of eggs in high temperature (39°C) can alter the metabolic rate of these embryos.

Thermal and spectroscopic studies of solid oxamate of light trivalent lanthanides

Solid-state LnL3·1.25H2O compounds, where L is oxamate and Ln is light trivalent lanthanides, have been synthesized. Simultaneous thermogravimetry and differential scanning calorimetry (TG-DSC), experimental and theoretical infrared spectroscopy, TG-DSC coupled to FTIR, elemental analysis, complexometry, and X-ray powder diffractometry were used to characterize and to study the thermal behavior of these compounds. The results led to information about the composition, dehydration, thermal stability, thermal decomposition, and gaseous products evolved during the thermal decomposition of these compounds in dynamic air atmosphere. The dehydration occurs in a single step and through a slow process. The thermal decomposition of the anhydrous compounds occur in a single (Ce), two (Pr), and three (La, Nd to Gd) steps with the formation of the respective oxides, CeO2, Pr 6O11, and Ln2O3 (Ln = La, Nd to Gd). The theoretical and experimental spectroscopic study suggests that the carboxylate group and amide carbonyl group of oxamate are coordinate to the metals in a bidentate chelating mode. © 2012 Akadémiai Kiadó, Budapest, Hungary.

Synthesis, characterization and thermal behavior of solid state compounds of heavy trivalent lanthanide succinates

Solid-state Ln-L compounds, where Ln stands for heavy trivalent lanthanides or yttrium(III) (Tb-Lu, Y) and L is succinate, have been synthesized. Simultaneous thermogravimetry and differential thermal analysis (TG-DTA), differential scanning calorimetry (DSC), infrared spectroscopy, TG-DTA coupled to FTIR, elemental analysis, X-ray powder diffractometry and complexometry were used to characterize and study the thermal behavior of these compounds. For the terbium to thulium and yttrium compounds, the dehydration, as well the thermal decomposition of the anhydrous compound occurs in two consecutive steps, while ytterbium and lutetium the dehydration occurs in a single step. The results also led to information about the ligand's denticity, thermal stability and thermal decomposition of these compounds. © 2013 Elsevier B.V.

Synthesis, characterization and thermal behaviour of solid-state compounds of folates with some bivalent transition metals ions

Solid-state M-L compounds, where M stands for bivalent Mn, Co, Ni, Cu and Zn and L is folate (C19H17N7O6), have been synthesized. Simultaneous thermogravimetry and differential scanning calorimetry (TG-DSC), X-ray powder diffractometry, infrared spectroscopy (FTIR), TG-DSC coupled to FTIR, elemental analysis and high-resolution continuum source flame atomic absorption spectrometry technique (HR-CS FAAS) were used to characterize and to study the thermal behaviour of these compounds. The results provided information concerning the composition, dehydration, thermal stability and thermal decomposition. © 2013 Akadémiai Kiadó, Budapest, Hungary.