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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:
June 27, 2017 - November 02, 2017
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Qualifier:
according to guideline
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Qualifier:
according to guideline
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
GLP compliance:
yes (incl. QA statement)
Type of method:
differential scanning calorimetry
Specific details on test material used for the study:
- Analytical purity: 100% (UVCB)
- Purity test date: 06 June 2017
- Lot/batch No.: 180517GT41
- Expiration date of the lot/batch: 31 December 2017
- Appearance: Beige pasty solid
- Storage: At room temperature
Decomposition:
ambiguous
Remarks:
Reaction and/or decomposition of the test item was observed during DSC experiments starting at a temperature of 200°C
Decomp. temp.:
200 °C
Remarks on result:
not determinable
Remarks:
A glass transition of the test item was observed at -59.2°C

RESULTS

Preliminary test

Starting at 250°C, the weight of the sample decreased significantly. At 270°C, the sample weight had decreased by 25%. After the experiment, a dark brown residue was observed on the lid of the sample container and a brown molten residue remained in the sample container (original colour: beige). The change of the colour indicated reaction and/or decomposition of the test item.

Main study

Experiment 1. During cooling, a glass transition was observed between -80°C and -50°C (results are archived in the raw data). During heating, a glass transition was observed between -75°C and -25°C. The inflection point of the glass transition was -59.139°C. An endothermic peak was observed starting at 200°C. The effect was due to reaction and/or decomposition of the test item. After the experiment, a brown molten residue remained in the sample container (original colour: beige) and a brown residue was observed on the lid of the sample container. The change of the colour indicated reaction and/or decomposition of the test item.

Experiment 2 (performed as a duplicate of Experiment 1 to obtain a second value for the glass transition but heating was stopped at a lower temperature). The inflection point of the glass transition was -59.207°C. After the experiment, the sample appeared unchanged.

The glass transition temperature was determined as the mean glass transition temperature of Experiment 1 (-59.139°C) and Experiment 2 (-59.207°C).

Conclusions:
No melting point was observed down to -90°C. A glass transition of the test item was observed at -59.2°C.
Executive summary:

The melting point of the test item was investigated in a GLP-compliant study performed in accordance with EU Method A.1 and OECD Guideline No. 102, using Differential Scanning Calorimetry (DSC). No melting point was observed down to -90°C. A glass transition of the test item was observed at -59.2°C.

Description of key information

The melting point of the test item was investigated in a GLP-compliant study performed in accordance with EU Method A.1 and OECD Guideline No. 102, using Differential Scanning Calorimetry (DSC). No melting point was observed down to -90°C. A glass transition of the test item was observed at -59.2°C.

Key value for chemical safety assessment

Additional information

The melting point of the test item was investigated in one GLP-compliant study performed in accordance with standard methods, without deviations. The study is considered as reliable (Klimisch 1) and was selected as key study for the endpoint.