Registration Dossier

Administrative data

Endpoint:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
key study
Study period:
08 March - 11 October 2016
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study

Data source

Reference
Reference Type:
study report
Title:
Unnamed
Year:
2016
Report Date:
2016

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 reports): JNJ-117676-AAA (T000263)
- Physical state: solid (powder)
- Appearance: White, slight beige amorphous, crystalline, micropowder
Specific details on test material used for the study:
- Batch n°: I15BB0491
- Analytical purity: 99.8% (base titration)
- Expiration date: 04 February 2021
- Storage condition: at room temperature

Results and discussion

Melting / freezing point
Key result
Melting / freezing pt.:
140 °C
Atm. press.:
1 013.25 hPa
Decomposition:
yes
Remarks:
A brown molten residue remained after the preliminary test and a yellow molten residue remained after the main test (up to 311°C), indicating reaction and/or decomposition.
Decomp. temp.:
> 250 °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 starting at 275°C. At 311°C the sample weight has decreased by 25%. After the experiment, a brown molten residue remained in the sample container (original colour: white to slightly grey powder). 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 showed an endothermic peak between 125°C and 150°C. The extrapolated onset temperature of the peak was 139.97°C. The effect was most likely obtained due to melting.

From 250°C a small exothermic followed by an endothermic effect was observed. The effect was most likely due to the start of reaction and/or decomposition of the test item. After the experiment, a yellow molten residue remained.

To investigate the melting peak between 125°C and 150°C, a repeated heating cycle was applied. The extrapolated onset temperature of the melting peak was 139.93°C. The melting temperature of T000263 was determined as the average melting temperature obtained from Experiment 1 and Experiment 2 and equals 140.0°C (413.1K).

Applicant's summary and conclusion

Conclusions:
The melting temperature of JNJ-117676-AAA (T000263) was determined at 140.0°C (413.1K) by using DSC.