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Melting point / freezing point

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Endpoint:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
weight of evidence
Study period:
2012-07-26 to 2012-08-01
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Qualifier:
according to guideline
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Version / remarks:
27 July 1995
Deviations:
no
Qualifier:
according to guideline
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
Version / remarks:
30 May 2008
Deviations:
no
GLP compliance:
no
Other quality assurance:
ISO/IEC 17025 (General requirements for the competence of testing and calibration laboratories)
Type of method:
differential scanning calorimetry
Key result
Melting / freezing pt.:
< -20 °C
Atm. press.:
1 013 hPa
Remarks on result:
other: No melting point was found between -150 and +50°C under these conditions. A glass transition was observed at -143°C.

The DSC measurements were performed twice. After cooling to -150°C at a rate of 2 K/min the sample was heated to 50°C at a rate of 5 K/min. The cooling as well as the heating curve show only a glass transition, indicating that the test item had solidified amorphously. The DSC thermograms are attached.

No other thermal effect from crystallisation or melting was registered upon further heating.

Conclusions:
No melting point was found between -150 and +50°C under the conditions of the study. A glass transition was observed at -143°C. The result is considered to be reliable.
Endpoint:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
weight of evidence
Study period:
2013-11-13 to 2013-11-14
Reliability:
2 (reliable with restrictions)
Rationale for reliability incl. deficiencies:
guideline study with acceptable restrictions
Remarks:
The study was conducted in accordance with OECD 102 but not in compliance with relevant quality management system.
Qualifier:
according to guideline
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
Deviations:
no
Qualifier:
according to guideline
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Version / remarks:
1995
Deviations:
no
Qualifier:
according to guideline
Guideline:
other: OECD 113 (1981) Screening test for thermal stability and stability in air
Version / remarks:
1981
Deviations:
no
GLP compliance:
no
Type of method:
thermal analysis
Remarks:
Differential Scanning Calorimeter
Key result
Melting / freezing pt.:
< -100 °C
Atm. press.:
1 013 hPa
Remarks on result:
other: Test item has no melting point above -100°C

Thermal stability (DSC measurement):

DSC measurement in a closed glass crucible showed an inconclusive base line. The DSC thermogram attached (figure 1).

Melting point/melting range (DSC measurement):

Two DSC measurements in aluminium crucibles with a hole showed no thermal effects in the temperature range of -100°C to room temperature. Therefore, the test item has no melting point above -100°C. The DSC thermograms attached (figure 2).

Conclusions:
The melting point of the substance was determined not to be above -100°C at 1013 hPa using a relevant test method. The result is considered to be reliable.

Description of key information

Melting point: <-1000°C at 1013 hPa (OECD 102)

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:
-100 °C

Additional information

Two measured melting/freezing point studies are available for the registered substance. In Mekelburger 2012, a glass transition temperature of -143°C at 1013 hPa was determined for the substance in accordance with OECD Test Guideline 102 (DSC - Differential Scanning Calorimetry) and in compliance with a known quality system (ISO 17025). Similarly, in Ahrens 2013, the result of thermal stability testing using DSC, indicates the test item has no melting point above -100°C (i.e. <-100°C) at 1013 hPa. The results were considered to be reliable and are used as weight of evidence.

In a secondary source to which reliability could not be assigned, a melting point of <0°C was reported for the substance.