The standard "ASTM D6604-00 Standard Practice for Glass Transition Temperatures of Hydrocarbon Resins by Differential Scanning Calorimetry" developed by the American Society for Testing and Materials (ASTM) describes an application for determining the glass transition temperatures of hydrocarbon (HC) resins by differential scanning calorimetry (DSC). This application is applicable to hydrocarbon (HC) resins as defined in the standard "ASTM D6640-21 Standard Practice for Collection and Processing of Soils Obtained in Core Barrel Samplers for Environmental Studies". The normal operating temperature range is from the cryogenic region to approximately 180 degrees. The temperature range can be extended.
For the purposes of this standard, differential scanning calorimetry (DSC) refers to a technique in which the difference in energy input to a substance and a reference material is measured as a function of temperature while the substance and the reference material are subjected to a controlled temperature program. Other terms and definitions related to thermal analysis are included in "ASTM E473-11a Standard Terminology for Thermal Analysis and Rheology".
This practice consists of heating or cooling the test material at a controlled rate, in a controlled atmosphere, and continuously monitoring, with a suitable sensing device, the difference in heat input between the reference material and the test material due to energy changes in the material. The absorption or release of energy marks a transition in the sample and causes a corresponding baseline shift in the heating or cooling curve.
Thermal analysis provides a rapid method for determining transition temperatures in hydrocarbon (HC) resins with these properties. This application is useful for both quality assurance and research.
The equipment used in these tests includes:
The main reagents used in these tests are:
Using the same heating rate that will be used for the samples, the temperature scale of the instrument is calibrated with appropriate standard reference materials covering the temperature range of interest.
When preparing a powder or granular sample, milling is avoided unless preliminary thermal cycling is performed. Milling or similar techniques for size reduction often cause thermal effects due to friction or orientation or both, thus altering the thermal history of the sample.
A sample weight appropriate for the material to be tested and the instrument used is used. In most cases, a sample weight of 10 mg to 20 mg is sufficient. Since milligram sample amounts are used, it is important to ensure that the samples are homogeneous and representative. Also, particle size has an effect on the transition temperatures detected. Therefore, particle size should be fairly consistent from sample to sample.
A preliminary thermal cycle is performed and recorded at a heating rate of 10 degree⁄min to a temperature high enough to erase previous thermal and strain history. An inert gas purge such as nitrogen should be used as the sample may react with oxygen during the temperature cycle, causing a false transition. An increase or decrease in the heating rate from that stated may alter the results.
This temperature is held for 10 minutes. Quench to 50 degrees below the expected transition temperature of interest. This temperature is held for 10 minutes. Heating is repeated on the same sample at a rate of 10 degrees per minute and the heating curve is recorded until all desired transformations are completed.
Among the numerous testing, measurement, analysis and evaluation studies that our organization has provided for businesses in various sectors, it also provides testing services defined in the standard “ASTM D6604-00 Standard application for glass transition temperatures of hydrocarbon resins by differential scanning calorimetry” with its trained and expert staff and advanced technological equipment.
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