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CHEM01200604004 Shri Sanyasinaidu Boddu - Homi Bhabha ...

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pulse frequency) as excitation sources for steady state and for lifetime measurements. Red<br />

sensitive PMT was used as the detector. Quantum yield was measured by using integrating<br />

sphere which is coated inside with BaSO 4 as a reflector.<br />

2.7.7. Thermal analysis: Thermal analysis methods are essential for understanding the<br />

compositional and heat changes involved during reaction. They are useful for investigating<br />

phase changes, decomposition, and loss of water or oxygen and for constructing phase<br />

diagrams.<br />

Thermo gravimetric analysis (TGA): In TGA, the weight of a sample is monitored as a<br />

function of time as the temperature is increased at a controlled uniform rate. Loss of water of<br />

crystallization or volatiles (such as oxygen, CO 2 , etc.) is revealed by a weight loss. Oxidation<br />

or adsorption of gas shows up as a weight gain.<br />

Differential thermal analysis (DTA): A phase change is generally associated with either<br />

absorption or evolution of heat. In DTA experiments, the sample is placed in one cup, and a<br />

standard sample (like Al 2 O 3 ) in the other cup. Both cups are heated at a controlled uniform<br />

rate in a furnace, and the difference in temperature (ΔT) between the two is monitored and<br />

recorded against time or temperature. Any reaction involving heat change in the sample will<br />

be represented as a peak in the plot of ΔT vs T. Exothermic reactions give an increase in<br />

temperature, and endothermic reaction leads to a decrease in temperature and the<br />

corresponding peaks appear in opposite directions.<br />

In the present study, thermo-gravimetric-differential thermal analysis (TG-DTA) of samples<br />

was carried out in platinum crucibles using a Setaram, 92-16.18 make TG-DTA instrument.<br />

The sample was heated under argon environment up to 1100°C at a heating rate of 10°C/min.<br />

53

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