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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
Study period:
19 FEB 2010 to 9 NOV 2010
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
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)
Deviations:
no
Qualifier:
according to guideline
Guideline:
other: EU Method A.2 (Boiling Temperature)
Deviations:
no
Qualifier:
according to guideline
Guideline:
other: OECD Guideline 103 (Boiling temperature)
Deviations:
no
GLP compliance:
yes
Type of method:
thermal analysis
Melting / freezing pt.:
-57.27 °C
Decomposition:
yes
Decomp. temp.:
116.34 °C

Run 1

A small endotherm with a peak at -57.45°C, possibly due to freezing/melting, was followed by an endotherm, with a peak at 121.53°C which was considered to be due to boiling.

Run 2

A small endotherm with a peak at -57.08°C, possibly due to freezing/melting, was followed by an endotherm, with a peak at 111.14°C which was considered to be due to boiling.

Thermal Data for Melting/Freezing Temperatures, Boiling/Decomposition Temperatures

Parameter

Run 1

Run 2

Mean

Endotherm 1

Onset (°C)

-59.24

-59.21

-59.23

Peak (°C)

-57.45

-57.08

-57.27

Enthalpy (J/g)

-54.82

-49.04

51.93

Endotherm 2

Onset (°C)

81.18

105.82

93.5

Peak (°C)

121.53

111.14

116.34

Enthalpy (J/g)

-272.31

-252.04

262.18

 

Conclusions:
The mean melting point was -57.27°C and the boiling point was 116.34°C.
Executive summary:

In run 1, a small endotherm with a peak at -57.45°C, possibly due to freezing/melting, was followed by an endotherm, with a peak at 121.53°C which was considered to be due to boiling.

In run 2, a small endotherm with a peak at -57.08°C, possibly due to freezing/melting, was followed by an endotherm with a peak at 111.14°C which was considered to be due to boiling.

Description of key information

In run 1, a small endotherm with a peak at -57.27°C was observed. In run 2, a small endotherm with a peak at -57.08°C was observed.

The mean of the two scans was given as the melting/freezing point.

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:
-57.27 °C

Additional information

The endpoint was determined in accordance with EU Method A.1 (Melting / Freezing Temperature) and OECD Guideline 102 (Melting point / Melting Range).

A sample was sealed in a vented aluminium DSC pan and scanned against a reference sample (an empty aluminium pan) from -60°C to 400°C at a heating rate of 10°C/minute after being held isothermally at -60°C for 15 minutes. Following examination of the results of this scan, a second test was performed. A second sample was scanned using the same temperature program.