Registration Dossier

Administrative data

Endpoint:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
key study
Study period:
27 Jul - 16 Aug 2016
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Remarks:
GLP 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:
EU Method A.1 (Melting / Freezing Temperature)
Version / remarks:
adopted in 2008
Deviations:
no
Qualifier:
according to
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Version / remarks:
adopted in 1995
Deviations:
no
GLP compliance:
yes (incl. certificate)
Remarks:
Department of Health, London, UK
Type of method:
differential scanning calorimetry

Test material

Reference
Name:
Unnamed
Type:
Constituent
Specific details on test material used for the study:
Storage conditions: room temperature in the dark

Results and discussion

Melting / freezing point
Key result
Atm. press.:
ca. 1 013 hPa
Decomposition:
yes
Decomp. temp.:
> 224.8 °C

Any other information on results incl. tables

Results

The thermographic data for determinations 1 to 6 are shown in the following table.

Table 2

Thermal event

Interpretation

Temperature

Determination 1

Determination 2

[°C]

[K]

[°C]

[K]

Sharp endotherm

Loss of volatiles

89.78

362.9

89.47

362.6

Sharp endotherm

Loss of volatiles / water

112.31

385.5

111.90

385.1

Sharp endotherm

Loss of volatiles

224.88

498.0

224.11

497.3

Thermal event

Interpretation

Temperature

Determination 3

Determination 4

[°C]

[K]

[°C]

[K]

Sharp endotherm

Loss of volatiles

89.54

362.7

89.54

362.7

Sharp endotherm

Loss of volatiles / water

111.96

385.11

112.07

385.2

Sharp endotherm

Loss of volatiles

225.19

498.3

225.15

498.3

Thermal event

Interpretation

Temperature

Determination 5

Determination 6

[°C]

[K]

[°C]

[K]

Broad endotherm

Loss of volatiles

70.66

343.8

68.32

341.5

 

 

Overall result: The test item does not melt or boil before decomposition occurs above 224.8 °C (498.0 K). As the test item did not melt, no melting point could be determined. As the test item decomposed, no value for boiling point could be determined.

 

Discussion

Determinations were carried out in pre-pierced crucibles from ambient to 450 °C in nitrogen and air at a rate of 20 °C/min to determine if there was a boiling point (determinations 1 to 4), the residues obtained were a black solid with approximately 50% loss in weight. Manually pierced crucibles were used for testing from ambient to 140 °C in air at a rate of 1 °C/min to establish if there was a melting point (determinations 5 to 6), the residues obtained were a yellow powder with approximately 10-15% loss in weight.

Similar thermographic profiles were obtained using air and nitrogen atmospheres. This indicated that the decomposition seen at 224.8 °C (498.0 K) was probably thermal and not oxidative.

Thermographic profiles (determinations 1 to 4) show transitions at 89.6 °C (362.7 K) and 112.1 °C (385.2 K), combine these transitions with the information from determinations 5 and 6, test item heated to only 140 °C, providing a residue after heating of a yellow powder with approximately 10-15% loss of weight for all determinations. A metal block determination providing visual investigation for this temperature region, showing that the test item began to “sweat” within the same temperature regions. The sample contains approximately 13% water, information supplied by sponsor, therefore these transitions can be concluded to be the loss of low boiling point volatiles and/or water within the test item.

Conclusion

The test item did not melt or boil before decomposition occurs above 224.8 °C (498.0 K). As the test item decomposed prior to melting, the melting and boiling points could not be determined.

Applicant's summary and conclusion