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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
Study period:
07 May 2015 - 03 Mar 2016
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Reason / purpose:
reference to other study
Reason / purpose:
reference to other study
Qualifier:
according to
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Version / remarks:
adopted in 1995
Qualifier:
according to
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
Version / remarks:
adopted in 2008
GLP compliance:
yes (incl. certificate)
Remarks:
Ministerium für Arbeit, Integration und Soziales des Landes Nordrhein-Westfalen, Düsseldorf, Germany
Type of method:
differential scanning calorimetry
Specific details on test material used for the study:
Storage conditions: at room temperature, tightly closed, dry
Remarks on result:
not determinable

Results
A preliminary thermogravimetric measurement was done over temperature range from room temperature to ca. 600 °C. Several mass loss steps were registered with a total mass loss of 74.2%. The residue looked black and incrusted. The course of the thermographic curve indicated the decomposition of the test item.

Test 1
Two DSC measurements were done in the temperature range 20 – 300 °C. The course of the heat flow curves showed two endothermic peaks (at max. 73 °C and 111 °C). This could be an indication for a two-phase melting. On the other hand the first peak could result from a phase transition (solid/solid) and the second one could result from the real melting. Further experiments were needed to clarify this.

Upon further heating the heat flow curves showed a very noisy course indicating decomposition prior to boiling. There was no evidence for a signal indicating boiling. Reweighing after the measurement showed that the sample had lost 55.5%/55.2% of its mass. The remaining residues looked yellow and melted.

Test 2
To clarify the melting behavior a second test with two different measurements was done.

A 1st measurement was made with heating until 80 °C (ca. the first endothermic peak from test 1). The peak at max. 74 °C could be seen again. After cooling down the residue looked visually unchanged and no mass loss could be measured.

A 2nd measurement was done with a first heating to 80 °C, cooling-down and a second heating-step again to 80 °C. here the peak at 74 °C could be seen too but during the second heating it could not be reproduced. Probably it is a matter of an irreversible phase transition and not a melting process. After cooling down the residue looked visually unchanged and no mass loss could be measured.

Conclusion: The test item has no melting point

Description of key information

No melting point determined (DSC, OECD 102)

Key value for chemical safety assessment

Additional information

DSC measurements showed endothermic peak at 73 °C. This peak could result from a irreversible phase transition (solid/soild) and is not a melting process. Therefore there is no melting point can be determined.