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Physical & Chemical properties

Melting point / freezing point

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Administrative data

Endpoint:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
key study
Study period:
10 November 2015 - 23 February 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 report): JNJ-38940642-AAA (T003010)
- Physical state: solid
- Appearance: white powder
Specific details on test material used for the study:
- Batch N°: I15AB0298
- Analytical purity: 99.7%
- Expiry date: 22 January 2017
- Storage condition: at room temperature

Results and discussion

Melting / freezing point
Key result
Melting / freezing pt.:
240.1 °C
Atm. press.:
1 013.25 hPa
Decomposition:
yes
Remarks on result:
other: A black molten residue remained after the preliminary test and a red/brown/dark yellow molten residue remained after the 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 at 275°C. At 399°C the sample weight has decreased by 25%. After the experiment, a black molten residue remained in the sample container (original colour: white). 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 50°C and 150°C. The effect was due to evaporation of volatile components. An endothermic peak followed by an exothermic peak between 225°C and 325°C was observed. The extrapolated onset temperature of the endothermic peak was 239.93°C. The exothermic effect was due to reaction and/or decomposition of the test item. Another exothermic effect started at 325°C. This effect was due to reaction and/or decomposition of the test item. After the experiment, a red/brown molten residue remained in the sample container.

To investigate the melting peak between 225°C and 325°C, a repeated heating cycle was applied. The extrapolated onset temperature of the melting peak was 240.28°C. After the experiment, a dark yellow molten residue remained in the sample container. The melting temperature of T003010 was determined as the average melting temperature obtained from Experiment 1 and Experiment 2 and equals 240.1°C (513.3K).

Applicant's summary and conclusion

Conclusions:
The melting temperature of JNJ-38940642-AAA (T003010) was determined at 240.1°C (513.3K) by using DSC.