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Physical & Chemical properties

Melting point / freezing point

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Reference
Endpoint:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
key study
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
other: Study performed according to international guidelines
Qualifier:
according to guideline
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Deviations:
no
Qualifier:
according to guideline
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
Deviations:
no
Principles of method if other than guideline:
In a measurement with differential scanning calorimetry (DSC) a sample of the test item and a reference material (identical crucible without the test item) are subjected to the same controlled temperature program. The difference in the temperatures of the test item and the reference material is recorded and applying a calibration function converted to a heat flow signal. When the sample undergoes a transition involving a change in enthalpy (endothermic on melting), that change is indicated by a departure from the base line of the heat flow record.

Thermogravimetry (TG) is based on continuous recording of mass changes of a sample as a function of temperature (with first derivative curve DTG).

Simultaneous Thermal Analysis (STA) generally refers to the simultaneous application of Thermogravimetry (TG) and Differential scanning calorimetry (DSC) to one and the same sample in a single instrument. The test conditions are perfectly identical for the TG and DSC signals (same atmosphere, gas flow rate, vapor pressure of the sample, heating rate, thermal contact to the sample crucible and sensor, radiation effect, etc.). The analyzability of the signals is improved, since two or more sets of information concerning sample behavior are always simultaneously available (differentiation between phase transformation and decomposition, between addition and condensation reactions, recognition of pyrolysis, oxidation, and combustion reactions, etc.).
GLP compliance:
yes (incl. QA statement)
Remarks:
DIN EN ISO/IEC 17025 certified
Type of method:
other: differential scanning calorimetry (DSC)
Specific details on test material used for the study:
Umicore h-powder
Melting / freezing pt.:
414 °C
Remarks on result:
other: (slightly overlapped by a small decrease in weight)

The DSC measurement was combined with a thermogravimetric (TG) measurement. The sample was purged 30 minutes with nitrogen before the start of the measurement (heating ramp). At the beginning the release of moisture is registered. Upon further heating the heat flow curves show one sharp endothermic peak with a peak maximum temperature at 425 °C and an extrapolated onset temperature of 414 °C, indicating the melting temperature at ambient pressure. The beginning of the melting peak is slightly overlapped by a small decrease in weight. Upon further heating decomposition is registered.

Conclusions:
Melting temperature is 414 °C

Description of key information

The melting point for this substance is 414 °C.

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:
400 °C

Additional information