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, with different purposes [ 3 – 6 ]. This study aimed to evaluate the thermal characterization of different salinities water by DSC-cooling. Experimental Samples The samples were collected in Serra
Abstract
A number of disintegrants are available on the market. They improve tablets’ disintegration. The objective of this work is the comparison of the technological quality parameters of disintegrants using different analytical techniques. Three batches of disintegrants and their binary mixtures (water:disintegrants) were investigated. Cooling experiments were used from –30 up to 200C. The data obtained showed calorimetric differences between the samples. In the binary mixtures water showed different crystallization behaviour from the one found in the literature. According to the results DSC technique helped the quality control of different disintegrants.
samples of indium ( T fus = 156.6 °C, Δ fus H = 3.266 kJ mol −1 ) and n -dodecane ( T fus = −9.65 °C, Δ fus H = 36.918 J mol −1 ). The temperature and heat flow uncertainties were estimated to be ±0.1 °C and ±0.05 mW, respectively. DSC cooling curves
Palm fat is one of the most commonly used fats in food industry. The main role of palm fat is to develop the desired texture of food products. Fat blends were developed to find the most appropriate mixture fitting the technological needs. In our work palm mid fraction (PMF) was mixed with anhydrous milk fat (AMF), goose fat (G), and lard (L) in a 1:1 ratio. Anhydrous milk fat represents fat consisting of a wide range of fatty acids. Goose fat is a soft, easily melting fat, and lard is characterized as animal fat with wide melting temperature interval. The measurements aimed to establish the miscibility of the fats and the effect of animal fats on the melting-solidification profile of palm mid fraction. SFC vs temperature curves, Differential Scanning Calorimetry (DSC) melting thermograms describe the melting profile of the samples. Isotherm crystallization by SFC vs time curves and DSC cooling thermograms were measured to characterize the solidification of pure fats and the blends. Since the SFC curves did not show crosspoints we concluded that fats blended in a 1:1 ratio were miscible. Anhydrous milk fat strongly modified the properties of palm mid fraction, the blend became similar to anhydrous milk fat. Goose fat had no strong modification effect on palm mid fraction and could be considered as a softening agent. The effect of lard was complex: melting and solidification behaviour of the blend differed from the characteristics of both parent fats.
Abstract
The first experimental evidence of the existence of the rigid amorphous fraction (RAF) was reported by Menczel and Wunderlich for several semicrystalline polymers. It was observed that the hysteresis peak at the glass transition was absent when these polymers were heated much faster than they had previously been cooled. In the glass transition behavior of poly(ethylene terephthalate) (PET), the hysteresis peak gradually disappeared as the crystallinity increased. At the same time, it was noted that the ΔC p of higher crystallinity PET samples was much smaller than could be expected on the basis of the crystallinity calculated from the heat of fusion. It was also observed that this behavior was not unique to PET only, but is characteristic of most semicrystalline polymers: the sum of the crystallinity calculated from the heat of fusion and the amorphous content calculated from the ΔC p at the glass transition is much less than 100% (a typical difference is ~20–30%). This 20–30% difference was attributed to the existence of the “RAF”. The presence of the RAF also affected the unfreezing behavior of the “mobile (or traditional) amorphous fraction.” As a consequence, the phenomenon of the enthalpy relaxation diminished with increasing rigid amorphous content. It was suggested that the disappearance of the enthalpy relaxation was caused by the disappearance or drastic decrease of the time dependence of the glass transition. To check the validity of this suggestion, the glass transition had to be also measured on cooling in order to overlay it on the DSC curves measured on heating. However, before this overlaying work could be accomplished, the exact temperatures on cooling had to be determined since the temperature of the DSC instruments that time could not be calibrated on cooling using the usual low molecular weight standards due to the common phenomenon of supercooling. Therefore, a temperature calibration method needed to be developed for cooling DSC experiments utilizing high purity liquid crystals using the isotropic → nematic, the isotropic → cholesteric, and other liquid crystal → liquid crystal transitions. After the cooling calibration was accomplished, the cooling glass transition experiments indicated that the glass transition in semicrystalline polymers is not completely time independent, because its width depends on the ramp rate. However, it was shown that the time dependence is drastically reduced, and the midpoint of the glass transition seems to be constant which can explain the absence of the enthalpy relaxation. The work presented here has led to a number of studies showing the universality of the rigid amorphous phase for semicrystalline polymers as well as an ASTM standard for DSC cooling calibration.
interval was defined as the difference between the average nucleation temperature and average solidus temperature determined on the first and second cooling. The tangents construction for the solidus temperature was done on the DSC cooling curve with the
.9 °C being too narrow, should be excluded from any analyzes. Fig. 1 DSC cooling and heating curves for pure cetane. The scanning rates were ±2 °C min −1 . Full , dashed , and dash-and-dotted lines show the
Treatment of water-induced curvature of the DSC heat flow rate signal
Applied to fractionated nucleation of polypropylene dispersed in water
-g-PP waterborne dispersions covering a three orders of magnitude range of particle sizes was produced, as reported previously [ 21 ]. The DLS determined PSD and the corresponding DSC cooling behavior are shown in Fig. 2a and b, respectively
heating curves for annealed samples in terms of increasing mass% Sn Fig. 5 Superimposed DSC cooling curves for annealed samples in terms of increasing mass% Sn
