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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:
09 October 2018 to 22 November 2018
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:
1995
Deviations:
no
Qualifier:
according to guideline
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
Version / remarks:
2016
Deviations:
no
Qualifier:
according to guideline
Guideline:
EPA OPPTS 830.7200 (Melting Point / Melting Range)
Version / remarks:
1998
Deviations:
no
GLP compliance:
yes
Type of method:
differential scanning calorimetry
Key result
Melting / freezing pt.:
< -80.1 °C
Atm. press.:
1 004 hPa
Decomposition:
no

Preliminary Test

- Starting at 150 °C, the weight of the sample decreased significantly. At 218 °C, the sample weight had decreased by 25 %.

- After the experiment it was observed that the test material was evaporated from the sample container.

 

Main Study

- During cooling no effects were observed. During heating an endothermic effect was observed between 150°C and 250°C. The extrapolated onset temperature of the effect was 219.294 °C. The endothermic effect was most likely obtained due to boiling of the test material. 

- After the experiment it was observed that the test material had evaporated from the sample container.

- In order to investigate the endothermic effect, a higher heating rate of 50 °C/minute was used in the Experiment 2. The extrapolated onset temperature was 220.324 °C. The endothermic effect had not shifted significantly to higher temperatures. It demonstrated that boiling of the test material caused the endothermic effect. After the experiment it was observed that the test material had evaporated from the sample container. Since a higher heating rate was used, the extrapolated onset temperature was not used in the calculation of the boiling point. 

- Experiment 3 was performed as a duplicate of Experiment 1. Similar results as in Experiment 1 were obtained. The extrapolated onset of the boiling effect was 218.868 °C. After the experiment it was observed that the test material had evaporated from the sample container.

- An additional investigation of the melting temperature of the test material was performed placing two subsamples of the test material for 25 hours at -21.0 ± 1.5 °C and at -80.1 ± 1.3 °C respectively. It was observed after storage that the test material was a liquid (-21.0 ± 1.5 °C) and a viscous liquid (-80.1 ± 1.3 °C). According to this it was concluded that the melting temperature of the test material is < -80.1°C (< 193.1K).

Conclusions:
Under the conditions of this study, the melting point of the test material was < -80.1 °C (< 193.1K).
Executive summary:

The melting point of the test material was investigated in accordance with the standardised guidelines OECD 102, EU Method A.1. and OPPTS 830.7200, under GLP conditions.

Under the conditions of this study, the melting point of the test material was < -80.1 °C (< 193.1K).

Description of key information

Under the conditions of this study, the melting point of the test material was < -80.1 °C (< 193.1K).

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:
-80.1 °C

Additional information

The melting point of the test material was investigated in accordance with the standardised guidelines OECD 102, EU Method A.1. and OPPTS 830.7200, under GLP conditions. The study was awarded a reliability score of 1 in accordance with the criteria set forth by Klimisch et al. (1997).

Under the conditions of this study, the melting point of the test material was < -80.1 °C (< 193.1K).