Registration Dossier

Administrative data

Endpoint:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
key study
Study period:
2017-01-31 to 2017-05-12
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 (incl. certificate)
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-7982559-AAA (T001329)
- Physical state: solid (powder)
- Appearance: Grey-brown powder
Specific details on test material used for the study:
- Batch n°: I14IB3639
- Analytical purity: 97.9% (based on HPLC)
- Expiration date: 2020-09-17
- Storage condition: at room temperature

Results and discussion

Melting / freezing point
Key result
Melting / freezing pt.:
197.8 °C
Atm. press.:
1 013.25 hPa
Decomposition:
yes
Remarks:
A brown molten residue remained after the preliminary and main test, indicating reaction and/or decomposition.
Decomp. temp.:
> 375 °C

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 at 400°C. At 422°C the sample weight has decreased by 25%. After the experiment, a dark brown molten residue remained in the sample container (original colour: grey brown). 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 obtained and showed an endothermic peak between 175°C and 225°C. The extrapolated onset temperature of the peak was 197.7°C. The effect was most likely obtained due to melting. A second endothermic peak was observed starting at 375°C due to reaction and/or decomposition of the test item. After the experiment, a brown molten residue remained. To investigate the melting peak between 175°C and 225°C, a repeated heating cycle was applied. The extrapolated onset temperature of the melting peak was 197.9°C. The melting temperature of T001329 was determined as the average melting temperature obtained from Experiment 1 and Experiment 2 and equals 197.8°C (471.0K).

Applicant's summary and conclusion

Conclusions:
The melting temperature of JNJ-7982559-AAA (T001329) was determined at 197.8°C (471.0K) by using DSC.