Registration Dossier

Administrative data

Endpoint:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
key study
Study period:
From 23 January 2017 to 16 March 2017
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:
EU Method A.1 (Melting / Freezing Temperature)
Version / remarks:
2008
Deviations:
no
Qualifier:
according to
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Version / remarks:
1995
Deviations:
no
Qualifier:
according to
Guideline:
EPA OPPTS 830.7200 (Melting Point / Melting Range)
Version / remarks:
1998
Deviations:
no
GLP compliance:
yes
Type of method:
differential scanning calorimetry

Test material

Reference
Name:
Unnamed
Type:
Constituent
Type:
impurity
Type:
impurity
Type:
impurity
Test material form:
solid: crystalline
Details on test material:
Appearance: white crystalline powder
Storage conditions: at room temperature protected from light

Results and discussion

Melting / freezing point
Key result
Melting / freezing pt.:
197.1 °C
Decomposition:
yes
Remarks on result:
other: Decomposition started during melting.

Any other information on results incl. tables

TGA EXPERIMENT (PRELIMINARY TEST)

From 190°C upwards the weight of the sample decreased significantly. At 197°C the sample weight had decreased by > 10%. At 293°C the sample weight had decreased by 25%.

DSC EXPERIMENT 1

-Endothermic peak between 175°C and 225°C (extrapolated onset temperature: 197.312°C). Based on the high purity of the substance and the observed weight loss in the TGA experiment, it was concluded that this effect was due to melting and reaction and/or decomposition.

-A second endothermic effect started from 250°C. This effect was due to decomposition and/or reaction of the substance.

-After the experiment, a dark orange molten residue remained in the sample container.

-DSC curve: see picture below.

DSC EXPERIMENT 2

- Extrapolated onset temperature of the endothermic melting/decomposition peak: 196.813°C.

- At the end of the experiment (at 225°C), there was a colourless molten residue in the sample container. From this it was concluded that melting and reaction/decomposition was the reason for this effect.

Applicant's summary and conclusion

Conclusions:
The melting temperature of the substance was determined to be 197°C. Reaction and/or decomposition started during melting.

Executive summary:

Differential Scanning Calorimetry (DSC) experiments were performed in a GLP study according to EC A.1, OECD 102 and OPPTS 830.7200.

The melting temperature of the substance was determined in duplicate obtaining a mean value of 197°C. Reaction and/or decomposition started during melting.