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]. Characterisation of the degree of crystallinity is conventionally investigated using techniques such as differential scanning calorimetry (DSC), X-ray analysis and density measurements. The kinetics of the crystallisation process are readily measured by DSC
. Differential scanning calorimetry (DSC) A DSC 822 e thermal analysis system (Mettler Toledo Instruments Inc. Switzerland) with nitrogen as purge (80 ml min −1 ) was used to investigate the isothermal crystallization kinetics as well as the non
calorimetry (DSC) data is analyzed with the help of the isoconversional methods of Kissinger–Akahira–Sunose (KAS) and Friedman. These isoconversional methods are extensively used for analysing non-isothermal decomposition, crystallization and degradation
any other metals, with MAP, due to limited prior geochemical interest in this mineral. The current study combines TG and differential scanning calorimetry (DSC) with evolved gas analysis by Fourier transform infrared spectroscopy (FT-IR) to
Abstract
Highly lipophilic basic drugs, the antiestrogens AE1 and AE2 shall be delivered transdermally. DSC as an additional tool in combination with classic investigation techniques should be used to clarify permeation enhancement. Skin treatment with pure solvents, polyethyleneglycol (PG) and dimethylisosorbide (DMI), slightly changed the phase transition temperatures. Formulations containing lauric acid markedly shifted these transitions to lower temperatures, indicating a lipid-fluidising action of lauric acid. In those cases an additional endothermic peak was observed around 40C, which is attributed to the melting of crystalline lauric acid. Since the DSC program started at -20C, it is very likely that lauric acid in the skin samples crystallized. A formulation of polyethyleneglycol and lauric acid leads to significantly higher deposition of lauric acid into the skin, in opposition to dimethylisosorbide/lauric acid formulation. These findings correspond to the results from our in-vitro permeation studies, where a significantly higher transdermal steady-state flux of lauric acid from polyethyleneglycol-formulation in comparison to dimethylisosorbide-formulation was observed. By this unique combination of polyethyleneglycol and lauric acid, the barrier is obviously modified in a way, which allows the highly lipophilic antiestrogens to permeate easily through the skin. So, from this formulation steady-state fluxes of AE-1 were observed, representing approximately the same value compared to the unhindered permeation through skin without stratum corneum. The grade of temperature shift on the skin lipids to lower temperatures can be correlated with softening effects and the enhancement potential of the formulation.
Abstract
A new method of calculation of parameters of enthalpy relaxation models is proposed. Regression analysis treatment compares the experimental and calculated values of relaxation enthalpy. The experimental values of relaxation enthalpy are obtained by numerical integration of the difference between the two DSC curves. Contrary to the overall shape of the DSC curve the integral values are not affected by particular heat flow conditions during the DSC experiment. The Narayanaswamy's numerical model based on the Kohlrausch—William—Watts relaxation function was used to calculate the theoretical values of relaxation enthalpy. The application of the proposed method on the DSC experimental data of enthalpy relaxation of As2Se3 is shown.
Kinetic analyses using simultaneous TG/DSC measurements
Part II: Decomposition of calcium carbonate having different particle sizes
Summary
The thermal decomposition of CaCO3was studied using simultaneous TG/DSC for two different ranges of particle size from the same source and a physical mixture of each. The difference in kinetic behavior was as expected qualitatively, but significantly different quantitatively. In addition, the mixture did not behave as a simple combination of its end members. These discrepancies are attributed to the problems associated with mass and thermal transport. The TG data again proved easier to fit than the DSC data.
Abstract
DSC purity analysis is based on thermodynamic phase diagrams for substances (purity ≥98%) which undergo a melting point. Impurities which have eutectic behaviour with the analyte are determined together. DSC purity analysis obtained from a single melting event of a 1–2 mg sample is, therefore, extremely attractive for the global assessment of eutectic impurities. The main advantages in early development lie in the very small amount of material necessary and the very fast analysis time. However, the DSC purity analysis cannot replace chromatographic methods which deliver specific individual levels of impurities. Furthermore, a complete validation of a DSC purity method is difficult and time consuming. Despite these limitations, DSC is the best support for the development of chromatographic methods, for purity profile and stability assessment during pharmaceutical development. Parameters of purity determination and validation aspects are discussed. Examples of use in pharmaceutical development are given.
Abstract
In pharmaceutical practice it is important and useful to know the crystallinity of materials and to monitor it during formulation development, production processes and storage. The purpose of this study was to assess the quantitative capability of DSC for determining crystallinity in crystalline/amorphous powder mixtures and to compare the accuracy of the DSC method with that of conventional powder X-ray diffraction. Alpha-lactose monohydrate was chosen as the model material. On the basis of this study it can be concluded, that DSC method can be applied safely for semiquantitative evaluation of the crystallinity of lactose samples consisting of an amorphous content higher than 20%.
Abstract
DSC studies of cracker mixtures of different compositions of potassium nitrate, sulphur and aluminum have shown some critical characteristics either with the increase or decrease in the composition of the components. Specifically, sulphur composition below 8% showed no exothermic activity. The studies revealed that a minimum of 11% to a maximum of 17% of sulphur is required for good cracking characteristics. The kinetics of decomposition of cracker mixture is carried out employing DSC multiple heating rate kinetic method. Increase in sulphur content decrease the energy of activation facilitating easy ignition of the cracker mixtures. Arrhenius parameters for cracker mixture decomposition are reported in this paper.
