Registration Dossier

Administrative data

Endpoint:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
key study
Study period:
08 July - 28 November 2016
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study

Data source

Reference
Reference Type:
study report
Title:
Unnamed
Year:
2017
Report Date:
2017

Materials and methods

Test guidelineopen allclose all
Qualifier:
according to
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Deviations:
no
Qualifier:
according to
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
Deviations:
no
Qualifier:
according to
Guideline:
EPA OPPTS 830.7200 (Melting Point / Melting Range)
Deviations:
no
GLP compliance:
yes
Type of method:
differential scanning calorimetry

Test material

Reference
Name:
Unnamed
Type:
Constituent
Test material form:
solid: particulate/powder
Details on test material:
- Name of test material (as cited in study report): JNJ-1580774-AAA (T000835)
- Physical state: solid powder
- Appearance: slight beige
Specific details on test material used for the study:
- Batch n°: I16BB1136
- Analytical purity: 99.3% (acid titration)
- Expiration date: 02 March 2017
- Storage condition: at room temperature

Results and discussion

Melting / freezing point
Key result
Melting / freezing pt.:
ca. 150.8 °C
Atm. press.:
1 013.25 hPa
Decomp. temp.:
ca. 150.8 °C
Remarks on result:
other: A light brown molten residue remained after the preliminary and a colourless molten residue after the main test, indicating reaction and/or decomposition.

Any other information on results incl. tables

Preliminary test

From the TGA curve it could be derived that the weight of the sample decreased significantly from 150°C. At 220°C the sample weight has decreased by 30%. After the experiment, a light brown molten residue remained in the sample container (original colour: white). The change of the colour indicated reaction and/or decomposition of the test item.

Main tests

In order to determine the melting more precisely, the DSC curve with a heating rate of 20°C/min was determined and showed an endothermic peak between 125°C and 175°C. The extrapolated onset temperature of the peak was 150.858°C. The effect was most likely obtained due to melting. After the experiment, a colourless molten residue remained. To investigate the melting peak between 125°C and 175°C, a repeated heating cycle was applied. The extrapolated onset temperature of the melting peak was 150.811°C. A colourless molten residue remained in the container after the experiment.

To investigate the melting peak a lower heating rate of 5°C/minute was applied in the Experiment 3. The extrapolated onset temperature of the melting peak was 137.301°C and the endothermic peak also started at the same temperature. The extrapolated onset temperature shifted to a lower temperature. It demonstrated that probably melting in combination with reaction and/or decomposition of the test item was the reason for the endothermic effect. After the experiment, a colourless molten residue remained in the sample container.

The melting temperature of T000835 was determined as the average melting temperature obtained from Experiment 1 and Experiment 2 and equals 150.8°C (424K).

Applicant's summary and conclusion

Conclusions:
The melting temperature (with decomposition) of JNJ-1580774-AAA (T000835) was determined at 150.8°C (424.0 K) by using DSC.