Differential Scanning Calorimetry Study

Luu Van Khue

Hanbat National University

DSC: The Technique

Differential Scanning Calorimetry (DSC) measures the temperatures and heat flows associated with transitions in materials as a function of time and temperature in a controlled atmosphere. These measurements provide quantitative and qualitative information about physical and chemical changes that involve endothermic or exothermic processes, or changes in heat capacity.

DSD is widely used in field of polymer materials.

Some Definitions
A calorimeter measures the heat into or out of a sample. A differential calorimeter measures the heat of a sample relative to a reference. A differential scanning calorimeterdoes all of the above and heats the sample with a linear temperature ramp. Endothermic heat flows into the sample. Exothermic heat flows out of the sample. Melting- The endothermic transition upon heating from a crystalline solid to the liquid state Crystallization- The exothermic transition upon cooling from liquid to crystalline solid

What DSC can tell you ?

Glass Transitions Melting and Boiling Points Crystallization time and temperature Percent Crystallinity Heats of Fusion and Reactions Specific Heat Oxidative/Thermal Stability Rate and Degree of Cure Reaction Kinetics Purity

DSC Components

DSC TA Q200: General DSC

DSC Accessories

Photocalorimeter Accessory (PCA)

DSC Pressure Cell

Heat Flow/Specific Heat Capacity

H = Cp T or in differential form
+

= Cp

thermal events

where: Cp = specific heat (J/gC) T = temperature (C) H = heat (J) dH/dt = heat flow (J/min.) dT/dt = heating rate (C/min.)

Cell Schematic Diagram

Heat-flux DSC

Measurement of HF and T

Furnace Temp.

Sample Temp.

Furnace Temp.

Inside of Heater Chamber

Typical DSC Transactions

Temperature (oC)

Exothermic up

Heat Flow (J/g)

Sample Preparation
Reference Pan Lid O-ring Pan

Sample Pan

High Pressure Pan

Operating of TA Q20
Turning on in order of: DSC Cell Run Computer Open gas flow Heating Method (NOTE: No equilibrate segment necessary if starting at or near ambient temperature) Ramp 10C/min. to 300C Cooling Method Equilibrate at 300C Ramp 10C/min. to 25C

Computer Analysis
Provides an interface between you and the analysis instruments Enables you to set up experiments and enter constants Stores experimental data Runs data analysis programs.

Thanks You for Your Kind Attention