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Soft Matter Facility (SoMF)

Texas A&M University College of Engineering

TA Instruments DSC 2500

 

 

1. Overview

  • DSC 2500 measures the difference in heat flow between a sample and an inert reference as both are subjected to a controlled temperature program.
  • When the sample undergoes a thermal event (melting, crystallization, glass transition, curing, oxidation, etc.), it absorbs or releases heat, detected as a change in heat flow.

2. Principle

  • The instrument maintains both the sample and reference at the same temperature.
  • Any temperature difference due to a thermal event causes the system to adjust the heat flow to restore equilibrium.
  • The heat flow difference (ΔQ/Δt) is directly proportional to the enthalpy change (ΔH) or specific heat capacity (Cp) of the sample.
  • Endothermic events (melting, dehydration) require additional heat input → positive heat flow.
  • Exothermic events (crystallization, oxidation) release heat → negative heat flow.

3. Data Interpretation

  • DSC measures the heat flow associated with thermal transitions as a function of temperature or time.
  • Typical DSC Results Include:
    • Heat Flow vs. Temperature Curve: Displays endothermic and exothermic transitions.
    • Thermal Events Identified:
      • Glass transition (Tg): Step change in baseline (no latent heat).
      • Crystallization (Tc): Exothermic peak indicating ordered structure formation.
      • Melting (Tm): Endothermic peak corresponding to phase change.
      • Thermal degradation: Exothermic or endothermic shifts at high temperatures.

4. Example Application

  • Pellet Thermal Behavior (1st Heat, As Received):
    • Lower curve values attributed to water plasticizing effect.
    • ΔCP at glass transition linked to amorphous phase content.
    • Large relative standard deviation likely due to processing conditions of as-received samples.
    • Melting temperatures (TM) and heats of fusion (ΔHF) show no clear correlation with fraction of added recycle.

Reference: TA469.pdf

5. Capabilities:

  • Direct heat capacity measurement
  • Glass transition Tg
  • Crystallization
  • Melting
  • Oxidation
  • Decomposition

6. Features:

  • Temperature range: -90 to 550°C
  • Temperature accuracy: ±0.025°C
  • Temperature precision: ±0.005°C
  • Enthalpy precision: ±0.04%

             

Publications involving the DSC system in the experimental conditions:

  • Study of the influence of alkene stereochemistry over thermal behaviour of the macromolecules
    • Stereocontrolled acyclic diene metathesis polymerization | Nature Chemistry
  • Study of the thermal performance of phase change materials embedded 3D printed objects
    • Thermal energy regulation with 3D printed polymer-phase change material composites | Matter
    • Printing Composites with Salt Hydrate Phase Change Materials for Thermal Energy Storage | ACS Applied Engineering Materials
  • Thermal performance of phase change materials embedded in 3D printed objects and polymer gels
    • Temperature- and creep-resistant Diels-Alder salogels for shape stabilization of salt hydrate phase change materials |Journal of Materials Chemistry A
    • Hybrid polymer salogels for reversible entrapment of salt-hydrate-based thermal energy storage materials |ACS Applied Engineering Materials
    • Strong, thermo-reversible salogels with boronate ester bonds as thermal energy storage materials |Journal of Materials Chemistry A
  • Determination of glass transition and bond dissociation temperature of stereoisomers of dynamic covalent Diels-Alder crosslinks
    • Stereochemical shape morphing in Diels-Alder polymer networks |Small
    • Supersonic puncture-healable and impact resistant covalent adaptive networks |Materials Horizons
    • Dynamic polymer network conductive composites: Low percolation threshold and Joule-heating induced network plasticity |Chemical Engineering Journal
    • Thermodynamics and stereochemistry of Diels-Alder polymer networks: role of crosslinker flexibility and crosslinking density |Macromolecules

 

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