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Methods

Thermal analyses

Thermal test methods such as differential thermal analysis (DSC), thermogravimetry (TGA), thermomechanical analysis (TMA) and dynamic mechanical analysis (DMA) are standard methods for material characterization in plastics testing. In general, these tests are used to analyze material changes as a function of temperature or time, whereby tests with controlled heating or cooling rates as well as isothermal and dynamic measurements are possible. The advantage is that comparatively little sample material or small sample sizes are required for all methods.

  • DSC is used to measure the change in heat flow of a material as a function of temperature or time. This method is used to determine melting points, crystallinity fractions, glass transitions, reaction enthalpies or the oxidation sensitivity of plastics.
  • TGA is used to determine the change in weight of a material as a function of temperature or time. In this way, filler content and, if necessary, the proportion of polymer/polymer mixtures as well as the thermal stability and degradation behavior of materials can be analyzed. 
  • TMA is used to determine the change in the dimensions of a material as a function of temperature in a spatial direction. The method enables high-precision measurements of the linear expansion coefficient, whereby tests can be carried out with both compressive and tensile loads.
  • DMA is used to analyze the viscoelastic behavior of a material as a function of temperature, time and/or frequency.
Martina Schubert
Project Manager | Special Services and Expert Reports
Würzburg
m.schubert@skz.de
Dr. Irene Reuther
Group Manager | Special services and expert reports
Würzburg
i.reuther@skz.de

Further details on the methods

Extract from our test methods

Accredited test methods

  • Differential scanning calorimetry (DSC) 
    e.g. according to DIN EN ISO 11357-2, DIN EN ISO 11357-3, DIN EN ISO 11357-6
  • Thermogravimetry (TGA) in accordance with DIN EN ISO 11358-1 and others
  • Thermomechanical analysis (TMA) in accordance with ISO 11359-2 and others
     

Non-Accredited test methods

  • Dynamic Mechanical Analysis (DMA)
What factors can influence the measurement results?

Sample preparation:
The correct preparation of the samples is crucial. Different stresses or excessive heat input can lead to different results.

Sample weight:
The weight of the sample can influence the sensitivity of the measurements. Sample weights that are too small or too large can lead to inaccurate results.

Heating rates and cooling rates:
The rate at which the temperature is increased or decreased can affect the measurement results.

Sample condition:
The physical condition of the sample, especially the sample history, can influence the results of a thermal analysis.

Transportation and storage conditions:
Any aging processes before and during storage of the sample can influence the results of a thermal analysis. 

Atmosphere:
The composition of the atmosphere can influence the measurement, which is why nitrogen is often used as an inert gas. In TGA, however, different gas atmospheres (air, nitrogen, oxygen) are specifically used to induce various degradation reactions.

Heat transfer and reaction kinetics:
In some cases, thermal events can occur simultaneously or in quick succession. The analysis of such superpositions requires special experimental procedures and knowledge in the evaluation of the measurement data.

Technical test equipment
  • Hitachi STA 7200 and Netzsch 209 F1 Iris
  • for thermogravimetric analysis
  • Netzsch 204 F1 Phoenix, Seiko DSC 220, and Seiko Exstar 6000
  • for differential thermal analysis
  • Hitachi TMA/SS7100 for thermomechanical analysis
  • Mettler Toledo DMA/SDTA861 for dynamic mechanical analysis
     
What are typical areas of application for thermal analysis?

Differential scanning calorimetry DSC: 
Identification of unknown polymers, determination of characteristic temperatures, analysis of polymer blends

Thermogravimetry TGA: 
Determination of filler content, formulation analysis, determination of thermal decomposition and degradation processes

Thermomechanical analysis TMA: 
Determination of linear expansion coefficients, identification of glass transitions

Dynamic mechanical analysis DMA: 
Characterization of viscoelastic properties, high-precision determination of glass transitions, characterization of temperature and frequency dependence of modulus and damping.
 

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