Registration Dossier

Administrative data

Endpoint:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
key study
Study period:
July 30, 2010 - February 24, 2011
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
other: GLP study conducted in compliance with international guidelines.

Data source

Reference
Reference Type:
study report
Title:
Unnamed
Year:
2011
Report Date:
2011

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
GLP compliance:
yes (incl. certificate)
Type of method:
other: Themal analysis and capillary test

Test material

Reference
Name:
Unnamed
Type:
Constituent
Test material form:
solid: particulate/powder
Remarks:
migrated information: powder

Results and discussion

Melting / freezing point
Melting / freezing pt.:
>= 220 °C
Decomposition:
yes
Remarks on result:
other: The test item started melting under decomposition at about 220 C

Any other information on results incl. tables

The DSC-curve of the preliminary test (heating rate of 20 °C/min from 25 °C to 400 °C) showed a first endothermic heat effect at 166.1 °C. A second endothermic heat effect was observed at 218.2 °C, followed by a third endothermic heat effect starting at 231.0 °C. After the experiment, the sample had lost 47.2% of its mass and a black, foamed and carbonized residue remained in the sample cup. In order to determine the first endothermic heat effect more precisely, a DSC-run was recorded between 140 °C and 200 °C with a heating rate of 10 °C/min. An endothermic heat effect was observed starting at 160.3 °C. After the experiment, the test item was still a powder. Thus, this endothermic heat effect is not due to melting of the test item. A further DSC-run was recorded between 140 °C and 240 °C with a heating rate of 10 °C/min. During this run, the first endothermic heat effect was observed at 159.6 °C and a second endothermic heat effect was observed at 210.7 °C. After the experiment, the sample lost 13.0% of its mass and a black melt remained in the sample cup. To clarify the results of the DSC runs more precisely, further tests were performed using the capillary tester and visual detection. In a first test a total of three samples were heated up from 25 °C to 400 °C with a heating rate of 20 °C/min. At 175 °C the samples became darker. At 200 °C some black spots were detected. At 220 °C the color of the test item was changed completely to black. At 226 °C the samples started melting while expanding. In a second test two samples were heated up from 140 °C to 300 °C with a heating rate of 10°C/min. From 170 °C to 217 °C the color of the samples became darker. At 220 °C the color of the samples was changed completely to black and the test item started melting.

Applicant's summary and conclusion

Conclusions:
With regard to the DSC-runs and the capillary tests, it can be concluded that the test item started melting under decomposition at about 220 C.
Executive summary:

The melting temperature of the test item has been determined according to OECD 102 and Council Regulation (EC) No. 440/2008, 30 May 2008, Part A, Methods for the determination of physico-chemical properties, A.1 in GLP. With regard to the DSC-runs and the capillary tests, it can be concluded that the test item started melting under decomposition at about 220 C.