Registration Dossier

Administrative data

Endpoint:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
key study
Study period:
7 March - 16 September 2017
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
Type of method:
differential scanning calorimetry

Test material

Reference
Name:
Unnamed
Type:
Constituent
Test material form:
liquid: viscous
Details on test material:
- Physical state: liquid (viscous)
- Appearance: clear viscous liquid
Specific details on test material used for the study:
- Batch n°: I16DB1991
- Analytical purity: 81.4 - 81.8%
- Expiration date: 7 June 2018
- Storage condition: at room temperature

Results and discussion

Melting / freezing point
Key result
Melting / freezing pt.:
-49.4 °C
Atm. press.:
1 013.25 hPa
Decomposition:
yes
Remarks:
A dark yellow to orange brown molten residue remained after the preliminary and main test, indicating reaction and/or decomposition.
Decomp. temp.:
> 150 °C
Remarks on result:
other: Glass transition temperature

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 225°C. At 288°C the sample weight has decreased by 25%. After the experiment, an orange brown molten 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

During cooling a glass transition (TG) of the test item was observed between -40°C and -80°C. During heating a glass transition (TG) was observed between -75°C and -25°C. The inflection point was -49.530°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, a dark yellow molten residue remained in the sample container.

 

Experiment 2 was performed to determine the duplicate inflection point of the glass transition (TG). The temperature program of the second experiment was stopped after the glass transition. The inflection point of the glass transition was -49.297°C. After the experiment, the residue remained in the sample container was unchanged.

 

The glass transition was determined as the average glass transition obtained from Experiment 1 (-49.530°C) and Experiment 2 (-49.297°C).

Applicant's summary and conclusion

Conclusions:
The glass transition temperature of JNJ-17337073-AAA (T001598) was determined at -49.4°C (223.7K) using DSC. No melting was observed.
Reaction and/or decomposition of JNJ-17337073-AAA (T001598) was observed during DSC experiment at temperatures of > 150°C (> 423K).