RESUMO
A weak acidic complex ester (CE) in solid form was prepared by a condensation reaction between very weak boric acid (BA: H3BO3) and (D)-mannitol (MA: C6H14O6) by the molar ratio of BA/MA = 2. A boron carbide (B4C) precursor was obtained from heating of the CE at 400 °C for 4 h. The precursor was pyrolyzed under argon flow in the interval of 1300-1550 °C for 4 h and at 1400 °C for 1-4 h, respectively. The materials were examined using several techniques such as X-ray diffraction analysis, thermal analysis, scanning electron microscopy, particle size distribution, and nitrogen adsorption/desorption. The optimum pyrolysis temperature and duration were 1400 °C and 4 h, respectively. The most crystalline B4C particles were distributed between 1 and 100 µm with a mean particle size of 20 µm. The specific surface area and specific pore volume were 13.5 m2 g-1 and 0.09 cm3 g-1, respectively. The size of the pores was between 2 and 36 nm with a mean size of 14 nm.
RESUMO
Two methods were proposed to calculate the thermodynamic parameters of porous ceramic compacts depending on their molar volume change with applied pressure and heating temperature, respectively. Molar volume of the porous α-alumina (α-Al2O3) compact was evaluated according to literature depending on both the applied pressure at room temperature and the heating temperature at atmospheric pressure. The isothermal compressibility coefficient, Gibbs energy, and work done on the compact by compression were calculated. The thermal shrinkage coefficient and activation energy as well as the change in enthalpy, entropy and Gibbs energy were calculated for partial sintering. The spontaneous nature of the treatments were discussed with respect to the obtained results.
RESUMO
The steel specimens were tempered in contact with uranium carbide powder by sodium bonding at 500, 600, 700, and 800 °C for 1000h. Carburizing zone of the specimens was determined by measuring of microhardness which is taken as a kinetic variable instead of the corresponding carbon content. Arrhenius equation was determined for the diffusion of carbon atoms in the steel by using the solution of Fick's second law. Temperature dependency of the activation enthalpy, Gibbs energy, and entropy was calculated from the transition state theory by an assumption that the carburizing occurs over an activated complex. Kinetic and thermodynamic for formation an activated complex were discussed depending on the obtained numerical values.
RESUMO
In this study, we used nano-smectite (SMT) and multiwall carbon nanotube (MWCNT) as a recognition surface over the disposable pencil graphite electrode for the low-level detection of ascorbic acid (AA) and acetyl salicylic acid (ACA). Firstly, nano-semectit was obtained by the purification of natural bentonite clay. XRD patterns and Scanning electron microscopy (SEM) were employed to ensure the purity of the bentonite samples. Pencil graphite rodes were immersed into suspensions of SMT, MWCNT or the both.The surface morphology of the sensor was investigated by cyclic voltammery (CV), electrochemical impedance spectroscopy (EIS) and SEM techniques. The effect of pH, percentage composition of modifiers, immobilization time, accumulation time and accumulation potential was optimized for reaching the best electroanalytical response for AA and ACA. The sensor developed proved to give good recovery, notable electro-catalytic activity and appropriately distant signals for the simultaneous determination of the analytes. Common contaminates, uric acid, l-cysteine, dopamine, glucose, Na+, Cl- and citric acid were investigated for their interference effects. Uric acid, citric acid and dopamine were found to interfere to some extent. The electrode exhibited wide working ranges and a fairly satisfactory detection limit of 0.096 and 0.241⯵M for AA and ACA, respectively. The electrode system proved to be practical for the analysis of pharmaceutical tablets and the recovery results are very satisfactory.
