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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:
From 01 July 2015 to 26 July 2016.
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Qualifier:
according to
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
Version / remarks:
2008
Deviations:
no
Qualifier:
according to
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Version / remarks:
1995
Deviations:
no
Qualifier:
according to
Guideline:
EPA OPPTS 830.7200 (Melting Point / Melting Range)
Version / remarks:
1998
Deviations:
no
GLP compliance:
yes
Type of method:
differential scanning calorimetry
Decomposition:
yes
Decomp. temp.:
225 °C
Remarks on result:
other: no melting/freezing point in the range -90 to 25°C
Remarks on result:
other: Glass transition at -62°C

TGA EXPERIMENT (PRELIMINARY TEST)

From 325°C upwards the weight of the sample decreased significantly. At 385°C the sample weight had decreased by 25%. After the experiment, a black brown molten residue remained in the sample container. Residue was observed on the lid of the sample container. The change of the colour indicated reaction and/or decomposition of the test substance.

 

DSC EXPERIMENT 1

During cooling, a glass transition was observed between -60°C and -80°C. During heating, a glass transition was observed between -75°C and -50°C. The inflection point of the glass transition was -61.76°C. From 225°C an exothermic followed by an endothermic effect was observed. The effect was due to reaction and/or decomposition of the test substance. After the experiment, a brown residue remained in the sample container.

 

DSC EXPERIMENT 2

Similar results as with Experiment 1 were obtained. The inflection point of the glass transition was -61.46°C. After the experiment, a brown residue remained in the sample container.

 

DSC EXPERIMENT 3

To investigate if the test substance did react during the glass transition the temperature program was stopped at 200°C. The inflection point of the glass transition was -61.64°C. After the experiment the sample appeared to have been unchanged, i.e. no decomposition and/or evaporation were observed. 

The glass transition temperature of the substance was calculated as the average from Experiment 1 (-61.76°C), Experiment 2 (-61.46°C) and Experiment 3 (-61.64°C): -62°C.

Conclusions:
PEMP product has no melting/freezing point in the range -90 to 25°C. The glass transition temperature of PEMP product was determined to be -62°C. Reaction and/or decomposition was observed at temperatures > 225°C.
Executive summary:

Differential Scanning Calorimetry experiments were performed in a GLP study according to EC A.1, OECD 102 and OPPTS 830.7200. The substance PEMP product is a liquid at room temperature. The substance has no melting/freezing point in the range -90 to 25°C. From three experiments, a mean glass transition temperature of -62°C was obtained. Reaction and/or decomposition was observed at temperatures > 225°C.

Description of key information

No melting/freezing point in the range -90 to 25°C (EC A.1, OECD 102, OPPTS 830.7200: DSC)

Glass transition temperature: -62°C.

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:
-20 °C

Additional information

The value of -20°C is the lower limit for melting/freezing point determination according to Column 2 of Annex VII to REACH and was therefore chosen as the key value for CSA.