Registration Dossier

Administrative data

Endpoint:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
key study
Study period:
2017-01-31 to 2017-06-06
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 (incl. certificate)
Type of method:
differential scanning calorimetry
Remarks:
glass transition temperature

Test material

Reference
Name:
Unnamed
Type:
Constituent
Test material form:
liquid: viscous
Details on test material:
- Physical state: Viscous liquid
- Appearance: Yellow to orange, clear liquid
Specific details on test material used for the study:
- Batch n°: I16HB3200
- Analytical purity: 83.7%
- Expiration date: 2017-07-25
- Storage condition: at room temperature

Results and discussion

Melting / freezing point
Key result
Melting / freezing pt.:
-47.3 °C
Atm. press.:
1 013.25 hPa
Decomp. temp.:
> 150 °C
Remarks on result:
other: Glass transition temperature
Remarks:
A orange yellow to orange brown 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 250°C onwards. At 294°C the sample weight has decreased by 25%. After the experiment, a 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

In order to determine the melting more precisely, the DSC curve with a cooling rate of -5°C/min was obtained and showed a glass transition (TG; temperature beyond which typically an amporphous solid softens) between -40°C and -80°C. During heating a glass transition (TG) was observed between -75°C and -25°C. The inflection point was -47.557°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 change of colour. After the experiment, a orange yellow 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-47.017°C. After the experiment, the residue in the sample container remained unchanged.

The glass transition was determined as the average temperature obtained from Experiment 1 (-47.557°C) and Experiment 2 (-47.017°C).

Applicant's summary and conclusion

Conclusions:
The glass transition temperature of JNJ-17337008-AAA (T001591) was determined at –47.3°C (225.9K) by using DSC. No melting was observed.