Recent developments in advanced thermal analysis: sample controlled thermal analysis

The determination of the key physical and chemical properties of a new material is essential.The melting point, glass transition temperature, the number and identification of the different phases it may have, and the temperatures at which they are formed are all of great value, not only in assessing its practical pharmaceutical potential but also as they can form the basis of many routine QC procedures

Thermal Studies on Rubidium Dinitramide

The present study has been carried out to investigate conflicting reports in the literature on the nature of the thermal decomposition of the energetic oxidant rubidium dinitramide in the liquid state. The techniques employed included DSC, simultaneous TG-DTA, simultaneous TG-mass spectrometry and thermomicroscopy. The measurements were supplemented by quantitative chemical analysis of the reaction products. The results showed that, following fusion at 106 °C, the overall decomposition proceeded in a single exothermic reaction stage forming a mixture of rubidium nitrate and rubidium nitrite in the molar ratio 1.2 : 1

Development and applications of sample controlled thermomicroscopy

Sample controlled thermal analysis techniques such as constant rate transformation analysis or stepwise isothermal analysis, where the transformation rate of the sample itself is used to control the experiment, are becoming increasingly important [1]. The measurements are normally carried out using changes in the sample mass, sample dimensions or in the evolved gas, as the property used to control the experiment, and enable reactions to be studied in greater detail than is possible using linear heating techniques. A new approach is described here where a thermomicroscopy system has been developed to enable the intensity of the light reflected or transmitted by the sample to be used as the controlling signal [2]

Determination of the temperature and enthalpy of the solid-solid phase transition of caesium nitrate by differential scanning calorimetry

The equilibrium temperature of the solid–solid phase transition of high purity caesium nitrate has been measured accurately by stepwise heating and by the extrapolation to zero heating rate method. A mean value of 154.3 ± 0.1 °C was obtained using two different heat flux DSC instruments. A value of 3.44 ± 0.04 kJ mol−1 was determined for the enthalpy of transition