Registration Dossier

Administrative data

Endpoint:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
key study
Study period:
07 March - 17 September 2017
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:
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
Type of method:
differential scanning calorimetry
Remarks:
glass transition temperature

Test material

Reference
Name:
Unnamed
Type:
Constituent
Test material form:
liquid
Details on test material:
- Name of test material (as cited in study reports): JNJ-42398681-AAA (T001589)
- Physical state: liquid
- Appearence: light brown
Specific details on test material used for the study:
- Batch n°: I16FB3011
- Analytical purity: 87%
- Expiration date: 14 March 2018
- Storage condition: at room temperature

Results and discussion

Melting / freezing point
Key result
Atm. press.:
1 013.25 hPa
Decomposition:
yes
Decomp. temp.:
> 150 °C
Remarks on result:
other: the glass transition temperature was determined to be -52.1°C
Remarks:
An orange residue remained after the preliminary and the first 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 225°C upwards. At 279°C the sample weight has decreased by 25%. After the experiment, a orange residue remained in the sample container (original colour: 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 was obtained and showed a glass transition temperature (TG) between -50°C and -80°C during cooling. During heating a glass transition of the test item was observed between -75°C and -25°C. The inflection point was -52.044°C. Starting at 150°C, the DSC curve showed an endothermic effect. The effect was most likely due to the start of reaction and/or decomposition, based on the results obtained by the preliminary test and the change of colour. After the experiment, an orange residue remained in the sample container.

 

Experiment 2 was performed to determine the duplicate inflection point of the TG. The temperature program of the second experiment was stopped after the glass transition. The inflection point of the glass transition was -52.243°C. After the experiment, the residue in the sample container remained unchanged.

 

The TGwas determined as the average temperature obtained from Experiment 1 (-52.044°C) and Experiment 2 (-52.243°C).

Applicant's summary and conclusion

Conclusions:
The glass transition temperature of JNJ-42398681-AAA (T001589) was determined at -52.1°C (221.0K) by using DSC. No melting was observed.