DIFFERENTIAL SCANNING CALORIMETRY (DSC)

Figure 1. DSC equipment.

Features

DSC can determine the melting point, crystallization temperature, and glass transition point of a sample from the change in heat energy caused by heating. It can also be used to determine crystallinity, purity, reaction rate, and crystallization rate.

Application Examples

Structural change due to heating of the following materials:

  • Rubber

  • Organic thin and thick films

  • Adhesives

  • Biopolymers

  • Metals

  • Ceramics

  • Inorganic materials such as those in lithium-ion rechargeable batteries

Principle

The heat-flux DSC continuously records the temperature difference between a reference substance and the sample when heated simultaneously.

From this temperature scan, the amount of heat, and the heat capacity of the transition and/or reaction can be obtained. The method differs from differential thermal analysis (DTA) in that the DSC temperature difference is designed to be proportional to the input difference of the thermal energy per unit time. As the temperature of the electric furnace (heater block) increases at a constant rate, the reference sample and the sample under measurement also increase at the same rate.

If an endothermic reaction occurs in the measurement sample, the temperature rise stops while the reaction occurs, whereas it continues in the reference sample. Hence, a temperature difference \(\mathrm{\Delta}T\) occurs between the two samples.

\(\mathrm{\Delta}T\) is alleviated by the heat flow flowing through the heat sensitive plate and the amount of heat per unit time (heat flow) flowing into the sample is proportional to the temperature difference between the two samples.

Therefore, by integrating \(\mathrm{\Delta}T\) with respect to time, the heat generated/absorbed during the reaction can be determined, and the heat capacity of the sample calculated.

Data example

Figure 2. DSC charts for a 1.130 mg In sample in an Al sample holder. The atmosphere was air, temperature rise rate 20 \(℃\ \text{min}^{- 1}\), and sampling rate 10 Hz. When the heat flow decreases (increases) by temperature, the reaction is endo (exo) thermic.

Data delivery formats

  • Graphs in the format exemplified by Figure 2 (PDF file)

  • Numerical data of the graphs (Microsoft® Excel® file)

Measurement specifications

Property

Value

Unit

Notes

Sample diameter

<4

mm

Al or Pt container

Temperature range

\[25 - 700\]

\[{^\circ}\text{C}\]

Outgassing may abort the measurement. Range must be below decomposition temperature

Heating rate

\[1 - 100\]

\[℃\ \text{min}^{- 1}\]

Constant temperature possible.

Measurement temperatures

\[\leq 500\]

\[℃\]

Air

\[\leq 700\]

Ar, N2

Items for enquiries

  • Purpose and scope of the analysis

  • Desired measurement atmosphere, temperature range, temperature rise rate

  • Sample information:

    1. Quantity, availability of pre-analysis samples

    2. Shape, condition, size, possibility of destructive testing

    3. Handling instructions

  • Delivery date:

    1. Desired delivery dates of preliminary and final results

    2. Handling instructions

  • Other relevant information

Caution

  • It may not be possible to measure samples that generate gases.

  • Contact us in advance to verify that the sample can be measured

  • This measurement is performed by MST’s subcontractor

Consultation and application for analysis

Our knowledgeable sales representatives will propose the most appropriate analysis plan.
Please feel free to contact us for a quote on the cost of your analysis.
For consultation and application, please use the inquiry form or call us.

Inquiry Form

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てむぞう&ますみん

Temuzo&Masumin