Registration Dossier

Administrative data

Endpoint:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
key study
Study period:
30 January 2018 - 20 April 2018
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study

Data source

Reference
Reference Type:
study report
Title:
Unnamed
Year:
2018
Report Date:
2018

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:
Physical state: solid
Appearance: White powder
Specific details on test material used for the study:
- Batch n°: I16DD2146
- Analytical purity: 99.7% (based on GC assay)
- Expiration date: 27 April 2018
- Storage condition: at room temperature

Results and discussion

Melting / freezing point
Key result
Melting / freezing pt.:
ca. 129.5 °C
Atm. press.:
1 013.25 hPa
Decomposition:
yes
Decomp. temp.:
> 250 °C
Remarks on result:
other: A a black charred residue remained after the preliminary and 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 at 325°C. At 334°C the sample weight has decreased by 25%. After the experiment, a black charred 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 obtained and showed an endothermic peak between 100°C and 150°C. The extrapolated onset temperature of the peak was 129.647°C. The effect was most likely obtained due to melting. After the experiment, a a brown molten residue remained. In order to investigate the endothermic peak,a second experiement was stopped directly after the melting peak. The extrapolated onset temperature of the melting peak was 129.403°C. The melting temperature of T003688 was determined as the average melting temperature obtained from Experiment 1 and Experiment 2 and equals 129.5°C (406.7K).

Applicant's summary and conclusion

Conclusions:
The melting temperature of JNJ-63757083-AAA (T003688) was determined at 129.5°C (406.7K) by using DSC.