Differential Scanning Calorymetry (DSC)

Thermal analysis methods, such as DSC, TG , DMA and TMA are suitable for determining the thermal properties of polymers and other materials. With its high information content, dynamic differential scanning calorimetry (DSC) is an indispensable test method in incoming goods control as well as in development, production, quality assurance, and damage analysis.

It can be used to analyze physical changes in state or chemical reactions associated with a change in enthalpy or specific heat capacity depending on temperature or time.

As a standard method in plastics characterization, the DSC method provides valuable information on parameters such as glass transition range, melting point or range, or the degree of crystallinity, which on the one hand are dependent on the material but are also induced by the mechanical and thermal conditions during the manufacturing process.

Principle

The principle of the method is based on measuring the heat flow between sample and reference. Both the sample crucible and the reference crucible (usually an empty aluminum crucible) are simultaneously subjected to a defined, linear temperature program, whereby the heat flows equally through the sample and the reference crucibles. If the heat capacity of the sample changes during the temperature program (heating/cooling) via phase conversion or chemical reaction, the result is a difference in heat flux which is proportional to the change in temperature of the sample and reference crucibles. As a result, a thermogram is obtained which reflects the exothermic or endothermic processes in the sample. As required, the sample room can be rinsed with various gases (nitrogen/oxygen/argon/air) to avoid or induce oxidation.

Our Services

  • Analysis of the smallest sample quantities of a wide range of materials
  • Determination of the conversion or reaction enthalpies and temperatures of endothermic (e.g. melting, glass transition, evaporation, sublimation, desorption, desolvation) and exothermic processes (e.g. crystallization, polymerization, chemisorption, combustion)
  • Freely-configurable temperature programs (–160 to 600 °C or RT to 1400 °C)
  • Heat flow calorimeter with automatic gas change

Applications

  • Determination of base and copolymer and identification of amorphous/semi-crystalline plastics by the characteristic conversion properties, such as melting point (range) and glass transition temperature
  • Detection of batch differences, determination of purity, phase conversions, adsorption and absorption, crystallization reactions, etc.
  • Determination of the influence of the processing conditions on the product properties, e.g. inherent tension
  • Investigation of curing and cross-linking reactions and post-cross linking (polymerization, polyaddition and polycondensation)
  • Analysis of photo-induced (light-induced) reactions in the material via UV irradiation (UV light curing of adhesives, varnishes, resin systems and coatings, study of UV stability – aging effects)
  • Determining the aging state and behavior (thermooxidative degradation) of polymer materials (oxidation induction time (OIT) and oxidation onset temperature (OOT))

DSC analysis of a multilayer film (PE-LLD, EVOH, PA6, PET)

Sample Requirements

  • Analysis of solid and liquid samples
  • Small sample quantities necessary (mg range)
  • Minimal sample preparation

Specifications

DSC 204 F1 Phoenix (Netzsch)
Temperature range: –160 to 600 °C
Heating rate: 0.001 to 200 K/min
Media: N2, O2, air

Extension:
Photo DSC attachment (OmniCure Series 2000)
Temperature range: –100 to 200 °C
Wavelength range: 320 to 500 nm
Output: ˜ 10 W/cm² (depending on the lamp)
Irradiation time: 0.2 to 1000 s
Aperture diameter: 8, 4, 2 mm

DSC 404 (Netzsch)
Temperature range: RT to 1400 °C
0,001 bis 200 K/min

Standard Excerpt

Accredited to:

DIN EN ISO 11357-1
Plastics – Differential scanning calorimetry (DSC)
Part 1: General principles
DIN EN ISO 11357-2
DIN EN ISO 11357-2 Plastics – Differential scanning calorimetry (DSC)
Part 2: Determination of glass transition temperature and step height
DIN EN ISO 11357-3
DIN EN ISO 11357-3 Plastics – Differential scanning calorimetry (DSC)
Part 3: Determination of temperature and enthalpy of melting and crystallization
DIN EN ISO 11357-6
Plastics – Differential scanning calorimetry (DSC)
Part 6: Determination of oxidation induction time (isothermal OIT) and oxidation induction temperature (dynamic OIT)

Based on:

DIN 53545
Determination of low-temperature behavior of elastomers
ISO 3146
Determination of melting behavior (melting temperature or melting range) of semi-crystalline polymers by capillary tube and polarizing-microscope methods, with reference to ISO 11357-3
ISO 11357-4
DSC – Determination of specific heat capacity
VW 50123
TGA + DSC – Thermoplastic elastomers
VW 44045
Polypropylene prefabricated parts
VDA 675116
DSC – Elastomer components in motor vehicles – Test methods for identification, cold characteristics

Contact

SGS INSTITUT FRESENIUS GmbH
Königsbrücker Landstr. 161
01109 Dresden

t +49 351 8841-200
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