Blog | Fauske and Associates, LLC

Measuring Heat Flow With Differential Scanning Calorimetry (DSC)

Written by AnnMarie Fauske | Nov 7, 2013 8:36:00 PM

By AnnMarie Fauske, Fauske & Associates, LLC

The Differential Scanning Calorimeter (DSC) measures the heat flow to or from a sample under controlled heating conditions. A small amount of sample (1-10 mg) is contained within a closed crucible and placed into a temperature controlled furnace. A second crucible is used as a reference. The sample is then heated by the temperature controlled furnace. The most commonly used method of temperature control is dynamic (or scanning) mode which utilizes a constant heating rate. Another mode of operation is isothermal mode and is used to maintain a constant temperature. In both of these modes, the heat flow to or from the sample is measured as a function of time and temperature.

DSC data can be used to assess the thermal hazard potential as well as evaluate material properties of a given sample. ASTM Standards commonly used for such evaluations are as follows:

 

  • ASTM E 537-12: Standard Test Method for the Thermal Stability of Chemicals by Differential Scanning Calorimetry
  • ASTM E 698-11: Standard Test Method for Arrhenius Kinetic Constants for Thermally Unstable Materials Using Differential Scanning Calorimetry and the Flynn/Wall/Ozawa Method
  • ASTM E 793-06: Standard Test Method for Heats of Fusion and Crystallization by Differential Scanning Calorimetry
  • ASTM E 794-06: Standard Test Method for Melting and Crystallization Temperatures by Thermal Analysis
  • ASTM E 928-08: Standard Test Method for Purity by Differential Scanning Calorimetry
  • ASTM E1269-11 Standard Test Method for Determining Specific Heat Capacity by Differential Scanning Calorimetry

Fauske & Associates, LLC (FAI) specializes in performing DSC tests on reactive chemical samples. High pressure crucibles are used to accommodate pressure generation due to both vapor and non-condensable gas. FAI is proud to partner with another industry leader, SWISSI Crucibles, to set standards for safety in thermal analysis. SWISSI is known worldwide for their crucibles and FAI is the exclusive North American Distributor for their patented two-piece gold and stainless steel high pressure crucibles (the M20 and F20 , respectively.)

Tested up to 200 bar (2900 psi) at 400°C (tested with supercritical water pressure) SWISSI Crucibles are:

  • Compatible
  • Reliable
  • Simple to use
  • Pressure resistant

SWISSI M20 and F20 Crucibles are:

  • Simple: New sealing principle (patented) using only two parts allows for lower sealing pressure
  • Reliable: New construction avoids undesirable surface effects of low viscosity solvents which can result in difficulties involving sealing and artefacts
  • Fast: Low time constant will allow higher heating rates and therefore higher throughput or permit a better signal resolution
  • Universal: Ready to be used with the market leaders’ DSC devices
  • Specifications: mass of 0.98g, height of 4.5mm, diameter of 7.0 mm, internal volume of 20μL

For more information regarding Thermal Stability, DSC or other process safety testing, please contact Jeff Griffin at griffin@fauske.com, 630-887-5278 or www.fauske.com