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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:
guideline study
Qualifier:
according to guideline
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
Qualifier:
according to guideline
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
GLP compliance:
no
Type of method:
thermal analysis
Remarks:
Differential Thermal Analysis (DTA) / Differential Scanning Calorimetry (DSC)
Melting / freezing pt.:
83.3 °C
Remarks on result:
other: mean of two determinations in a closed crucible and of two determinations in an open crucible with perforated lid

Thermal behaviour and stability by DTA/DSC:

At room temperature the substance is solid and crystalline.

Between 25 °C and 450 °C two endothermic effects were visible. A steep signal was detected between approx. 80 °C - 90 °C indicating a melting point. For the second endothermic effect between approx. 110 °C - 150 °C a further melting range was assumed.

Between approx. 175 °C and 315 °C significant exothermic effects were observed. After the heating process a brownish residue remains in the crucible indicating decomposition of the test item.

Melting point:

Measurements with closed crucible and open crucible show a steep endothermic phase.

The melting process was found to be not reversible. A one-time heated sample was cooled down and heated up again to 100 °C. The thermal effect could not be detected anymore.

After the heating and cooling down process a waxy creamy white residue remains in the crucible.

Conclusions:
The melting point of the test item was determined to be 83.3 °C.
Executive summary:

To determine the melting point of the test item a differential thermoanalysis method (DTA) was used which conforms with the procedure Test method A.1, "Determination of the melting point", described in the EC-Guideline.

The weighed sample was closed up in a crucible made of aluminium, placed in a DTA/DSC-system and adjusted to 60 °C. The sample was then heated up to 100 °C (heating rate 1 K/min). In comparison with an inert sample (empty crucible) the temperature difference and the heat effect were recorded.

Measurements with closed crucible and open crucible show a steep endothermic phase. The endothermic signal was evaluated to give the following melting points (mean value): 83.3 °C.

The melting process was found to be not reversible. A one-time heated sample was cooled down and heated up again to 100 °C. The thermal effect could not be detected anymore.

After the heating and cooling down process a waxy creamy white residue remains in the crucible.

Description of key information

The melting point of the test item was determined to be 83.3 °C.

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:
83.3 °C

Additional information

To determine the melting point of the test item a differential thermoanalysis method (DTA) was used which conforms with the procedure Test method A.1, "Determination of the melting point", described in the EC-Guideline.

The weighed sample was closed up in a crucible made of aluminium, placed in a DTA/DSC-system and adjusted to 60 °C. The sample was then heated up to 100 °C (heating rate 1 K/min). In comparison with an inert sample (empty crucible) the temperature difference and the heat effect were recorded.

Measurements with closed crucible and open crucible show a steep endothermic phase. The endothermic signal was evaluated to give the following melting points (mean value): 83.3 °C.

The melting process was found to be not reversible. A one-time heated sample was cooled down and heated up again to 100 °C. The thermal effect could not be detected anymore.

After the heating and cooling down process a waxy creamy white residue remains in the crucible.

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