Registration Dossier

Administrative data

Endpoint:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
key study
Study period:
01 February 2018 - 13 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:
- Name of the test material (as cited in study reports): JNJ-63757109-AAA (T003690)
- Physical state: solid (powder)
- Appearance: white to slightly yellow power
Specific details on test material used for the study:
- Batch n°: I17BD0751
- Analytical purity: 99.9 % (titration)
- Expiration date: 24 February 2019
- Storage condition: at room temperature

Results and discussion

Melting / freezing point
Key result
Melting / freezing pt.:
253.4 °C
Atm. press.:
1 013.25 hPa
Decomposition:
yes
Decomp. temp.:
> 275 °C
Remarks on result:
other: A black charred and black molten residue remained after the preliminary and the first main test respectively, 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 300°C. At 353°C the sample weight has decreased by 25%. After the experiment, a black charred residue remained in the sample container (original colour: slightly yellow). 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 225°C and 275°C followed by an exothermic effect starting at 275°C.

The extrapolated onset temperature of the peak was 253.549°C. The effect was most likely obtained due to melting. After the experiment, a black molten residue remained. The colour change indicated reaction and/or decomposition of the test item.

To investigate the endothermic peak, a repeated heating cycle was applied up to 200°C and thus stopped directly after the endothermic peak. The extrapolated onset temperature of the melting peak was 253.343°C. After the experiment a colourless molten residue remained in the sample container which demonstrated that melting was the reason for the endothermic effect.

The melting temperature of T003690 was determined as the average melting temperature obtained from Experiment 1 and Experiment 2 and equals 253.4°C (526.6K).

Applicant's summary and conclusion

Conclusions:
The melting temperature of JNJ-63757109-AAA (T003690) was determined to be 253.4°C (526.6K) by using DSC.