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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:
22 January - 04 May 2016
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Qualifier:
according to guideline
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Deviations:
no
Qualifier:
according to guideline
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
Deviations:
no
Qualifier:
according to guideline
Guideline:
EPA OPPTS 830.7200 (Melting Point / Melting Range)
Deviations:
no
GLP compliance:
yes
Type of method:
differential scanning calorimetry
Specific details on test material used for the study:
- Batch n°: M15BB1451
- Analytical purity: 98.8% (base titration)
- Expiration date: 30 January 2021
- Storage condition: at room temperature
Key result
Melting / freezing pt.:
92.2 °C
Atm. press.:
ca. 1 026 hPa
Decomposition:
yes
Decomp. temp.:
>= 200 - <= 250 °C

Preliminary test

From the TGA curve it could be derived that the weight of the sample decreased significantly starting at 225°C. At 299°C the sample weight had decreased by 25%. After the experiment, a brown molten residue remained in the sample container (original colour: white to slight beige). The change of the colour indicated reaction and/or decomposition of the test item.

Main tests

The DSC curve with a heating rate of 20°C/min showed an endothermic peak between 75°C and 125°C. The extrapolated onset temperature of the peak was 92.11°C. The effect was most likely obtained due to melting. A second endothermic effect was observed between 225°C and 350°C due to decomposition of the test item between 200 and 250°C. After the experiment, a brown molten residue remained.

To investigate the melting peak between 75°C and 125°C, a repeated heating cycle (up to 120°C) in combination with a hermetically sealed sample pan (in order to investigate the boiling point) was applied in the 2nd experiment. The extrapolated onset temperature of the melting peak was 91.90°C. After the experiment, a brown molten residue remained in the sample container.

In the third experiment, the sample was heated up to 120°C. The extrapolated onset temperature of the melting peak was 92.55°C. The visual inspection showed that the test item had melted.

A fourth experiment was performed as a duplicate of experiment 1. Similar results were obtained. The extrapolated onset of the melting peak was 92.29°C, while the second endothermic peak is most likely caused by reaction and/or decomposition starting between 200 and 250°C. After the experiment, a brown molten residue remained in the sample container.

The melting temperature of T000750 as the average melting temperature from Experiment 1 (92.11°C), Experiment 2 (91.90°C), Experiment 3 (92.55°C) and Experiment 4 (92.29°C) was determined to be 92.2°C (365.4K) by using DSC. Reaction and/or decompostion of T000750 was observed between 200 and 250°C (between 473.2 and 523.2K).

Conclusions:
The melting temperature of JNJ-130806-AAA (T000750) was determined to be 92.2°C (365.4K) by using DSC.
Reaction and/or decomposition was observed starting at a temperature between 200 and 250°C (between 473.2 and 523.2K).

Description of key information

A GLP study was performed according to OECD guideline 102, EU Method A.1 and EPA OPPTS 830.7200 without deviations (Brekelmans, 2017). The melting point of T000750 was determined to be 92.2°C 365.4K) by using DSC.

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:
92.2 °C

Additional information

Reaction and/or decomposition was observed during DSC experiments starting at a temperature between 200 and 250°C (between 473.2 and 523.2K).