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Differential Scanning Calorimetry Part 1: Principles and technology (1) Pierre LE PARLOUËR Therm@l Consulting leparlouer@thermalconsulting.com
Differential Scanning Calorimetry Part 1: Principles and technology (2) Pierre LE PARLOUËR Therm@l Consulting leparlouer@thermalconsulting.com
Definition of the DSC technique according to ICTAC (1) • What is ICTAC? • Definition of DSC according to ICTAC For more information see www.ictac.org
Definition of the DSC technique according to ICTAC (1) • What is ICTAC? • Definition of DSC according to ICTAC For more information see www.ictac.org
Principle of the thermal analysis technique (1) • Equipment • Heating block • Sample and inert reference material • Thermocouple • Measurement Heating
Principle of the thermal analysis technique (2) Heating of the sample and the inert reference material at a constant heating rate Difference between sample and inert reference material temperatures Record of the furnace, sample and inert reference material temperatures
Principle of the thermal analysis technique (2) Heating of the sample and the inert reference material at a constant heating rate Difference between sample and inert reference material temperatures Record of the furnace, sample and inert reference material temperatures
Endothermic and exothermic effects (1) Heat Flux EXO Temperature (°C) heating cooling ENDO Time (sec) See also evitherm Thermal Analysis/Definitions
Endothermic and exothermic effects (1) Which peak direction for the endothermic and exothermic effecst? Heat Flux EXO Temperature (°C) heating cooling ENDO Time (sec) See also evitherm Thermal Analysis/Definitions
A typical DSC curve with endothermic and exothermic effects What are the detected endothermic effects? What are the detected exothermic effects? The DSC curve (3) See also evitherm Thermal Analysis/Applications
A typical DSC curve with endothermic and exothermic effects What are the detected endothermic effects? What are the detected exothermic effects? The DSC curve (3) See also evitherm Thermal Analysis/Applications
Diagram of a DSC apparatus (1) • A DSC apparatus is built around : - a differential detector - a signal amplifier - a furnace - a temperature controller - a gas control device - a data acquisition device See also evitherm Thermal Analysis/Equipment suppliers
Diagram of a DSC apparatus (2) • A DSC apparatus is built around : - a differential detector - a signal amplifier - a furnace - a temperature controller - a gas control device - a data acquisition device See also evitherm Thermal Analysis/Equipment suppliers
Mathematical expression of the calorimetric signal (1) • Expression of the heatflux from the reference side • Expression of the heatflux from the sample side
Mathematical expression of the calorimetric signal (2) • Expression of the heatflux from the reference side • Expression of the heatflux from the sample side
Mathematical expression of the calorimetric signal (1) • Determination of the difference of thermal power exchanged through the thermal resistance (R) between the furnace and each container • Final equation giving the mathematical expression of the calorimetric signal
Mathematical expression of the calorimetric signal (2) • Determination of the difference of thermal power exchanged through the thermal resistance (R) between the furnace and each container • Final equation giving the mathematical expression of the calorimetric signal
The calorimetric curve (1) Base line Heat Flux (mW) Tf Temperature (°C) Ti Area under the peak corresponding to the heat effect (expressed in mJ) Time (sec) See also evitherm Thermal Analysis/Units
The calorimetric curve (2) Base line Heat Flux (mW) Tf Temperature (°C) Ti Area under the peak corresponding to the heat effect (expressed in mJ) Time (sec) See also evitherm Thermal Analysis/Units
Specific heat determination (1) • Definition of the Specific heat capacity Cp • How to measure Cp from the DSC curve • Cp experiments 3 2 1
Specific heat determination (2) • Definition of the Specific heat capacity Cp • How to measure Cp from the DSC curve • Cp experiments 3 2 1
Different calorimetric principles (DSC, calorimetry) Heat Flux Plate DSC Heat Flux Calvet DSC Power compensated DSC See also evitherm Thermal Analysis/Measurement methods
Principle of a plate-type DSC (1) • Description of a plate-type DSC • Measurement of the heat flow • Experimental conditions • Calibration Schematic of a plate-shape DSC sensor
Principle of a plate-type DSC (2) • Description of a plate-type DSC • Measurement of the heat flow • Experimental conditions • Calibration Schematic of a plate-shape DSC sensor
Principle of the power compensated DSC (1) • Description of a power compensated DSCC • Measurement of the heat flow • Experimental conditions • Calibration
Principle of the power compensated DSC (2) • Description of a power compensated DSCC • Measurement of the heat flow • Experimental conditions • Calibration
Principle of a Heat Flux CALVET DSC (1) • Calvet principle • Description of a heat flux Calvet DSC • Measurement of the heat flow • Experimental conditions • Calibration
Principle of a Heat Flux CALVET DSC (2) • Calvet principle • Description of a heat flux Calvet DSC • Measurement of the heat flow • Experimental conditions • Calibration