Registration Dossier

Administrative data

Endpoint:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
key study
Study period:
August to november 2017
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Justification for type of information:
The determination was carried out by differential scanning calorimetry, using a procedure designed to be compatible with Method A.1 Melting/Freezing Temperature of Commission Regulation (EC) No440/2008 of 30 May 2008 and Method 102 of the OECD Guidelines for Testing of Chemicals, 27 July
1995

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)
Qualifier:
according to
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
GLP compliance:
yes (incl. certificate)
Type of method:
differential scanning calorimetry

Test material

Reference
Name:
Unnamed
Type:
Constituent
Test material form:
solid: crystalline
Details on test material:
White powder
Specific details on test material used for the study:
Batch18114773 - purity > 99.5%
The temperature accuracy of the DSC was checked prior to testing with indium and zinc. These were within defined tolerances and the DSC was therefore considered acceptable for use.
Aliquots of test item (see following table) were placed in pierced crucibles and were subjected to a thermal program from 80 to 180 °C at 1 °C/min.
The appearance of the samples (residue) was recorded after the test.

Results and discussion

Melting / freezing point
Key result
Melting / freezing pt.:
> 145.9 - < 146.9 °C

Any other information on results incl. tables

 Thermal event     Interpretation        Temperature (°C)
 Determination 1  Determination 2
 Endotherm 1 extrapolated onset temperature Extrapoled onset of possible polymeric changes  137.6   137.68
   Endotherm 1 extrapolated onset temperature  Extrapoled onset of melting 146.42   146.44

On thermal analysis, two distinct, consistent endothermic events were observed, possibly indicative of a polymorphic nature to the test item. A visual assessment of the melting characteristics of the test item, performed using a metal block apparatus, confirmed a broad melting temperature range for the test item starting at 143 °C. Additional cyclic differential scanning calorimetry, utilizing a temperature program of 125 to 142 °C at 1 °C/min, reduce temperature to 120 °C with a second heating to 142 °C at 1 °C/min was carried out. This cyclic determination showed only a single peak, allowing the first endotherm at approximately 137 °C to be excluded as an endotherm associated with melting.

Applicant's summary and conclusion

Conclusions:
The melting point of the test item has been determined to be 146.4 ± 0.5°C (419.6 ± 0.5 K).
Executive summary:

The melting point of the test item has been determined to be 146.4 ± 0.5°C (419.6 ± 0.5 K). Testing was performed by a differential scanning calorimetry procedure designed to be compatible with Method A.1 Melting/Freezing Temperature of Commission Regulation (EC) No 440/2008 of 30 May 2008 and Method 102 of the OECD Guidelines for Testing of Chemicals, 27 July 1995.