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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 June 12, 2017 to September 20, 2017
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Qualifier:
according to guideline
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
Version / remarks:
2008
Deviations:
no
Qualifier:
according to guideline
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Version / remarks:
1995
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.:
>= 9 - <= 29.4 °C
Decomposition:
yes
Decomp. temp.:
> 50 °C

TGA EXPERIMENT (PRELIMINARY TEST)

Starting at 100°C, the weight of the sample decreased significantly: 25% weight loss at 316°C and 70% weight loss at 440°C.

After the experiment, a dark brown molten residue remained in the sample container. The change of the colour indicated reaction and/or decomposition of the test substance.

 

DSC EXPERIMENT 1

During cooling two exothermic peaks were observed between 25°C and -25°C, most probably due to crystallisation of the test substance. During heating three endothermic peaks were observed between -25°C and 50°C directly followed by a broad endothermic effect starting at 50°C. The peak max temperature of the first peak was 9.329°C and of the last peak was 29.370°C. The endothermic effects were most likely obtained due to melting of the test substance. After the experiment, a light yellow molten residue remained in the sample container. 

DSC EXPERIMENT 2

In order to investigate whether reaction and/or decomposition of the test substance did already occur during melting, Experiment 2 was stopped at 50°C. Again, endothermic peaks were observed between -25°C and 50°C. The peak max temperature of the first peak was 8.979°C and of the last peak was 19.627°C. After the experiment, an off-white molten residue remained in the sample container. It demonstrated that melting was the reason for the endothermic effect and that reaction and/or decomposition of the test substance did not occur at temperatures up to 50°C. 

DATA HANDLING

The melting temperature was determined as a melting range obtained from the lowest peak max of the first melting temperature (9.0°C) and the highest peak max of the last melting temperature (29.4°C).

Conclusions:
Under the study conditions, from duplicate experiments, the melting range was established between 9.0°C and 29.4°C. Reaction and/or decomposition of the substance occurs at temperatures above 50°C.
Executive summary:

A study was conducted to determine the melting point of the test substance according to OECD 102 Guideline, EU Method A.1 and OPPTS 830.7200. A melting range instead of a well defined melting temperature was determined. Under the study conditions, from duplicate experiments, the melting range was established between 9.0°C and 29.4°C. Reaction and/or decomposition of the substance occurs at temperatures above 50°C (Reingruber, 2017).

Description of key information

The melting point was determined according to OECD Guideline 102, EU Method A.1 and OPPTS 830.7200 (Reingruber, 2017).

Key value for chemical safety assessment

Additional information

The melting range: 9.0°C - 29.4°C. Reaction and/or decomposition: >50°C.

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