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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:
20 October 2011 - 23 February 2012
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
other: GLP guideline study
Qualifier:
according to guideline
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Version / remarks:
27 July 2995
Deviations:
no
Qualifier:
according to guideline
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
Version / remarks:
31 May 2008
Deviations:
no
GLP compliance:
yes
Type of method:
differential scanning calorimetry
Key result
Melting / freezing pt.:
< -80 °C
Atm. press.:
1 013.325 hPa

Preliminary test:

From 300 °C upwards the weight of the sample decreased significantly. At 340 °C the sample weight had decreased by 25%. After the experiment, grey/black residue was observed on the lid of the sample container and a black residue remained in the sample container (original colour: pale yellow). The change of the colour indicated reaction and/or decomposition of the test substance.

Main study:

During heating, a small endothermic effect was observed between -25 °C and 25 °C. The effect was most likely obtained due to melting of water present in the test substance. The extrapolated onset temperature of the peak was -3.28 °C. This conclusion was also based on an exothermic effect (crystallization of water) that was observed during cooling between -30 °C and -60 °C (results are archived in the raw data). After melting of water, a broad endothermic effect was observed between 50 °C and 250 °C followed by reaction and/or decomposition of the test substance (exothermic effect starting at 250 °C). The first effect was possibly due to evaporation of water and/or other volatile impurities of the test substance.

After the experiment, a light yellow residue was observed on the lid of the sample container and in the sample container (original colour: pale yellow). The change of the colour indicated reaction and/or decomposition of the test substance. The second experiment was performed to obtain a duplicate measurement on the effects observed below 250 °C.

Similar results to the first experiment were obtained. The extrapolated onset of the melting peak of water was -4.11 °C. After the experiment, the test substance colour was unchanged, only a small aliquot of substance was evaporated.

To further investigate the melting temperature of the test substance two samples of the compound were stored overnight in the freezers at -20 °C and -80 °C. It was observed after storage that the test substance was still a liquid (white paste) in both freezers. According to this observation, it was concluded that the melting temperature of the test substance is < -80 °C.

Description of key information

The melting point of the test substance is < -80 °C (OECD 102, DSC).

Key value for chemical safety assessment

Additional information