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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:
21 June 2016 to 29 June 2016
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
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
GLP compliance:
yes (incl. QA statement)
Type of method:
differential scanning calorimetry
Key result
Melting / freezing pt.:
>= 53.2 - <= 83.87 °C
Decomposition:
ambiguous

Test A

- The test was conducted in an open aluminium crucible. The sample was observed to undergo an endothermic event (melting) from 66.19.7 °C (-3.87.0 J.g^-1). A second endothermic event was then observed to commence from *276.76 °C which had a heat of melting of -109.40.g^-1. An exothermic event was then observed at 376.60 °C, with a heat of decomposition of 491.08 J.g^-1.

- The value of 276.76 °C marked with an asterisk was taken from evaluation DSC81816A2 as the software incorrectly estimated the onset temperature in evaluation DSC81816A due to the presence of a sharp peak in the endotherm.

 

Test B

- The test was conducted in an open aluminium crucible. The sample was observed to undergo an endothermic event (melting) from *53.20 °C (-10.26.0 J.g^-1). A second endothermic event was then observed to commence from *218.93 °C which had a heat of melting of -171.47.g^-1. An exothermic event was then observed at 376.27 °C, with a heat of decomposition of 315.54 J.g^-1.

- The values 53.20 and 218.93 °C marked with an asterisk were taken from evaluation DSC81816B2 as the software incorrectly estimated the onset temperature in evaluation DSC81816B. This was due to the peak observed in the overall outline of the endotherm.

- A sample of the test material was analysed using a capillary melting point apparatus. This confirmed that the first endotherm was due to the melting point.

- The melting point was therefore 53.20 - 83.87 °C (range of two runs). The melting point is reported as a melting range from the lowest onset value to the highest peak value.

Conclusions:
Under the conditions of this study the melting point of the test material was in the range 53.20 - 83.87 °C. The melting point is reported as a melting range from the lowest onset value to the highest peak value.
Executive summary:

The melting point of the test material was investigated in accordance with the standardised guidelines OECD 102 and EU Method A.1, under GLP conditions using differential scanning calorimetry.

Duplicate tests were conducted in an open aluminium crucible.

In the first test the sample was observed to undergo an endothermic event (melting) from 66.19.7 °C (-3.87.0 J.g^-1). A second endothermic event was then observed to commence from 276.76 °C which had a heat of melting of -109.40.g^-1. An exothermic event was then observed at 376.60 °C, with a heat of decomposition of 491.08 J.g^-1.

In the second test the sample was observed to undergo an endothermic event (melting) from 53.20 °C (-10.26.0 J.g^-1). A second endothermic event was then observed to commence from 218.93 °C which had a heat of melting of -171.47.g^-1. An exothermic event was then observed at 376.27 °C, with a heat of decomposition of 315.54 J.g^-1.

A sample of the test material was analysed using a capillary melting point apparatus. This confirmed that the first endotherm was due to the melting point.

The melting point was therefore 53.20 - 83.87 °C (range of two runs). The melting point is reported as a melting range from the lowest onset value to the highest peak value.

Description of key information

Under the conditions of this study the melting point of the test material was in the range 53.20 - 83.87 °C, the melting point is reported as a melting range from the lowest onset value to the highest peak value.

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:
53.2 °C

Additional information

The melting point of the test material was investigated in accordance with the standardised guidelines OECD 102 and EU Method A.1, under GLP conditions using differential scanning calorimetry. The study was awarded a reliability score of 1 in accordance with the criteria set forth by Klimisch et al. (1997).

Duplicate tests were conducted in an open aluminium crucible.

In the first test the sample was observed to undergo an endothermic event (melting) from 66.19.7 °C (-3.87.0 J.g^-1). A second endothermic event was then observed to commence from 276.76 °C which had a heat of melting of -109.40.g^-1. An exothermic event was then observed at 376.60 °C, with a heat of decomposition of 491.08 J.g^-1.

In the second test the sample was observed to undergo an endothermic event (melting) from 53.20 °C (-10.26.0 J.g^-1). A second endothermic event was then observed to commence from 218.93 °C which had a heat of melting of -171.47.g^-1. An exothermic event was then observed at 376.27 °C, with a heat of decomposition of 315.54 J.g^-1.

A sample of the test material was analysed using a capillary melting point apparatus. This confirmed that the first endotherm was due to the melting point.

The melting point was therefore 53.20 - 83.87 °C (range of two runs). The melting point is reported as a melting range from the lowest onset value to the highest peak value.

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