Registration Dossier

Administrative data

Endpoint:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
key study
Study period:
16 Sep - 07 Nov 2016
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:
2017

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:
solid: particulate/powder
Details on test material:
- Name of test material (as cited in study reports): JNJ-40064973-AAA (Isonicotinezuur)
- Physical state: solid (powder)
- Appearance: white powder
Specific details on test material used for the study:
- Batch n°: M15HB3488
- Analytical purity: 98.9%
- Expiration date: 30 July 2020
- Storage condition: at room temperature

Results and discussion

Melting / freezing point
Key result
Atm. press.:
1 022 hPa
Decomposition:
no
Sublimation:
yes
Subl. temp.:
308.8 °C
Remarks on result:
other: The test item was observed to evaporate from the sample container

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 301°C the sample weight has decreased by 25%. After the experiment, a colourless residue remained in the sample container (original colour: white).

Main tests

In order to determine the melting more precisely, the DSC curve with a heating rate of 20°C/min was obtained which showed a small exothermic peak which was followed by an endothermic peak from 225.0°C. Based on the weight loss of the preliminary test and the sample consistency which remained the same, the effect is most likely obtained due to evaporation/sublimation of the test item. However, in Experiment 2 which was performed with a higher end temperature, no exothermic effect was observed. Only an endothermic peak from 225°C (extrapolated onset 308.647°C). After the experiment, the test item seems to be evaporated from the conainer, which may be due to sublimation. A third experiment was carried out to determine the duplicate evaporation/sublimation temperature. The extrapolated onset temperature of the endothermic peak in Experiment 3 was 308.919°C, similar to Experiment 2.  Afterwards, it was observed that the test substance was evaporated from the sample container.    

The evaporation/sublimation temperature was determined as the average extrapolated onset temperature of the endothermic peaks obtained from experiment 2 (308.647°C) and experiment 3 (308.919°C)

Applicant's summary and conclusion

Conclusions:
The evaporation/sublimation temperature of JNJ-40064973-AAA (Isonicotinic acid) was determined at 308.8°C (581.9K) by using DSC.