This research aimed to reduce the variability on the data obtained from differential scanning calorimetric (DSC) analysis of the isothermal crystallization kinetics of cocoa butter.
To enable transformation of the DSC crystallization peak to a sigmoid crystallization curve, the DSC peak area has to be integrated. Usually, the start and end points of the crystallization peak are determined visually. The result of this visual determination appeared to be very much dependent on the operator, but also differed considerably when the same operator performed the integration several times. By proposing an objective calculation algorithm to determine the start and end points of integration, the variability caused by the operator during the integration procedure could be eliminated. Furthermore, sample preparation and the DSC heating protocol to melt the sample prior to crystallization were studied. Three heating protocols (65 °C for 15 min, 65 °C for 30 min and 80 °C for 15 min) were compared and it was shown that holding at 65 °C for 15 min was sufficient to eliminate any influence of sample history. Two different sample preparation procedures were compared and it appeared that a change in sample preparation procedure had a significant influence on the measured crystallization process. It is thus important to keep this method constant to eliminate the variability caused by it. 相似文献
Luminescence characteristics of a number of undoped and variously doped PbWO4 crystals were studied at 0.4–400 K by the time-resolved spectroscopy and compared with those of ZnWO4,CdWO4 and PbMoO4 crystals. Two types of green emission centres are detected in PbWO4 crystals. The centres of the first type are responsible for the low-temperature 2.3–2.4 eV emission observed under excitation around 3.90–3.95 eV. The structure and parameters of their relaxed excited states were determined. It was concluded that the origin of defects responsible for the green emission of the first type could vary for different crystals. The centres of the second type with the emission around 2.5 eV appear in crystals containing oxygen vacancies after the thermal destruction of Pb+-WO3 centres at T>180 K. Decomposition of the exciton and various defect-related states was also studied, and activation energies of this process were calculated. 相似文献
Tin and titanium ferrocyanides were studied as adsorbents for alkali metal ions, viz., 134Cs and 22Na, which represent radioactive wastes. The ferrocyanides were prepared in granular form. The tin version contained 11.2% water, while the titanium version contained 17.7% water. The exchange capacities for Cs+ and Na+ in the hydrated tin version were about 1.5 and 0.7 meq/g, respectively, while those in the titanium version were 2.2 and 1.2 meq/g, respectively. Drying at 250°C decimated those capacities. The diffusional time constant of Cs+ at 25°C, determined via Fick's second law, was of order of magnitude 1 × 10–3 s–1, though there were minor differences due to particle size and the form of ferrocyanide. Similarly, the effective diffusivity was of order of magnitude 1 × 10–8 cm2/s. The titanium version responded slightly faster than the tin version. Likewise, equilibrium measurements in mixtures with sodium nitrate, potassium nitrate, or uranium oxide, showed that the titanium version exhibited significantly greater selectivity for Cs+ than did the tin version. Unfortunately, tests of complete elution of the Cs+ from the ferrocyanides were mostly disappointing. Work continues on that subject. 相似文献
The kinetics of four sorption systems, Cu/tree fern, Pb/tree fern, AB9/activated clay and BR18/activated clay have been studied based on the assumption of a pseudo-second order rate law. Pseudo-isotherms using the pseudo-second order kinetic expression constant have been developed to describe the four liquid-solid sorption systems. The experimental results have been analyzed using a pseudo-Langmuir and a pseudo-Redlich-Peterson isotherm. Both isotherms were found to represent the measured sorption data well. According to the evaluation using the pseudo-Langmuir equation, the monolayer sorption capacities were obtained to be 13.9, 46.6, 124 and 105 mg g–1 for copper, lead, AB9 and BR18 respectively. 相似文献