Registration Dossier

Administrative data

Endpoint:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
key study
Study period:
22 December 2017 - 07 June 2018
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study

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
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
Version / remarks:
2016
Deviations:
no
Qualifier:
according to guideline
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Version / remarks:
1995
Deviations:
no
Qualifier:
according to guideline
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

Constituent 1
Chemical structure
Reference substance name:
(8R,9S,10R,13S,14S,17R)-17-ethynyl-17-hydroxy-13-methyl-1,2,8,9,10,11,12,14,15,16-decahydrocyclopenta[a]phenanthren-3-one
EC Number:
608-630-3
Cas Number:
31528-46-8
Molecular formula:
C20H24O2
IUPAC Name:
(8R,9S,10R,13S,14S,17R)-17-ethynyl-17-hydroxy-13-methyl-1,2,8,9,10,11,12,14,15,16-decahydrocyclopenta[a]phenanthren-3-one
Test material form:
solid: particulate/powder
Details on test material:
Appearance: Off-white powder
Test item storage: At room temperature

Results and discussion

Melting / freezing point
Key result
Melting / freezing pt.:
242.9 °C
Decomposition:
yes
Decomp. temp.:
> 275 °C

Any other information on results incl. tables

Two experiments were performed to investigate the melting and boiling behaviour of the substance.

DSC EXPERIMENT 1

An endothermic peak was observed between 200°C and 250°C followed by an exothermic effect starting at 275°C (see the illustration below). The extrapolated onset temperature of the first peak was 242.969°C. The endothermic effect was most likely caused by melting of the test item. The exothermic effect was probably caused by reaction and/or decomposition of the test item.

After the experiment, a dark brown molten residue remained in the sample container (original colour: off-white). The change of the colour indicated reaction and/or decomposition of the test item. 

 

DSC EXPERIMENT 2

In order to investigate the melting peak, in Experiment 2 heating was stopped directly after the melting effect.  The extrapolated onset temperature was 242.887°C. After the experiment, a white molten residue remained in the sample container. It demonstrated that melting was the reason for the endothermic effect.

 

DATA HANDLING

The melting temperature was determined as the mean melting temperature of Experiment 1 and Experiment 2.

Applicant's summary and conclusion

Conclusions:
The melting temperature of the substance was determined to be 242.9°C.
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 242.9°C.

Reaction and/or decomposition of the substance was observed at temperatures > 275°C.