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Differential Scanning Calorimetry
Differential scanning calorimetry (DSC) is a thermal analysis technique used to characterize a variety of temperature-dependent physical and chemical changes in a material.
- Direct method of measuring reaction rate and some reaction kinetics
- Direct method of measuring heat capacity and detecting material thermal transitions
- Oxidation analysis, volatile material characterization, thermal degradation experiments, and solvent loss measurements are not supported as they can permanently damage the instrument
- Upper temperature limit must be lower than material decomposition temperature
DSC curve measured from Poly(ethylene terephthalate) (PET) packaging. First upward-oriented (endothermic) peak shows cold crystallization; next negative (exothermic) peak corresponds with the material melting point (annotated). Glass transition occurred near 70 C as a step in the heat-flow baseline.
From: Center for Advanced Materials Analysis in Oregon (CAMCOR)
- No volatile samples
- Only samples with known decomposition temperature can be tested
(TGA recommended as a preliminary test / screening method to validate sample viability for DSC)
TA Instruments SDT-Q600
- Temperature Range: ambient to 1500 °C
- Ramp Rate: 1 °C/min up to 30 °C/min
- Temperature Accuracy: 1 °C
- Air or N2 atmosphere options
DSC instruments measure the amount heat transferred (exothermic (heat produced) and endothermic (heat required) between a sample and its environment as the overall temperature of the system is modulated / ramped.
The sample is placed in a small pan and sealed. To increase the precision of the measurement, the system simultaneously measures heat flux in both the sample of interest, and an adjacent reference (a “blank,” or empty) pan.
After the energy transfer in the reference is subtracted from the specimen signal, one is left with a DSC curve that quantitatively reflects the temperature dependence of numerous thermal events. Characteristic features in a DSC curve correspond to certain thermodynamic processes, as well as exothermic and endothermic chemical and physical transitions. These transitions can include include: recrystallization, softening and phase changes.
By identifying these, it is possible to quantify the temperatures at which they occur, often allowing identification of the material (s) and to calculate additional, correlated thermal properties.
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