13-ethyl-11-methylene-gon-4-ene-3,17-dione

Melting point / freezing point

Administrative data

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

22 June 2020 - 29 July 2020

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Cross-reference

Reason / purpose for cross-reference:

reference to same study

Reference

Endpoint:

boiling point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

22 June 2020 - 29 July 2020

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Reason / purpose for cross-reference:

reference to same study

Qualifier:

according to guideline

Guideline:

EU Method A.2 (Boiling Temperature)

Version / remarks:

2016

Deviations:

no

Qualifier:

according to guideline

Guideline:

OECD Guideline 103 (Boiling Point)

Version / remarks:

1995

Deviations:

no

Qualifier:

according to guideline

Guideline:

EPA OPPTS 830.7220 (Boiling Point / Boiling Range)

Version / remarks:

1996

Deviations:

no

GLP compliance:

yes

Type of method:

differential scanning calorimetry

Key result

Decomposition:

yes

Decomp. temp.:

300 °C

Remarks on result:

other: no boiling up to decomposition

see IUCLID 4.2 melting point

Conclusions:

Boiling of the substance was not observed below the temperature at which reaction and/or decomposition started (i.e. at 300°C). Based on this, the substance has no boiling temperature.

Executive summary:

see IUCLID 4.2 melting point

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2020

Materials and methods

Test guideline

Test guideline 1

Qualifier:

according to guideline

Guideline:

EU Method A.1 (Melting / Freezing Temperature)

Version / remarks:

2016

Deviations:

no

Test guideline 2

Qualifier:

according to guideline

Guideline:

OECD Guideline 102 (Melting point / Melting Range)

Version / remarks:

1995

Deviations:

no

Test guideline 3

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

Test material information

Constituent 1

Reference substance name:

(3aS,3bS,9aR,9bS,11aS)‐11a‐ethyl‐10‐methylidene‐1H,2H,3H,3aH,3bH,4H,5H,7H,8H,9H,9aH,9bH,10H,11H,11aH‐cyclopenta[a]phenanthrene‐1,7‐dione

Cas Number:

54024-17-8

Molecular formula:

C20 H26 O2

IUPAC Name:

(3aS,3bS,9aR,9bS,11aS)‐11a‐ethyl‐10‐methylidene‐1H,2H,3H,3aH,3bH,4H,5H,7H,8H,9H,9aH,9bH,10H,11H,11aH‐cyclopenta[a]phenanthrene‐1,7‐dione

Test material form:

solid: particulate/powder

Details on test material:

Storage Conditions: In refrigerator (2-8°C)

Results and discussion

Melting / freezing point

Key result

Melting / freezing pt.:

156.2 °C

Any other information on results incl. tables

TGA EXPERIMENT (PRELIMINARY TEST)

The weight of the sample decreased significantly at temperatures above 325°C: 25% decrease at 413°C and 70% decrease at 458°C.

Appearance of the sample after the experiment: an orange brown molten residue.

The change of colour is an indicator for reaction and/or decomposition of the test item.

 

DSC EXPERIMENT 1

An endothermic effect was observed between 125°C and 175°C followed by a broad endothermic effect starting at 300°C. The extrapolated onset temperature of the first effect was 156.149°C. The endothermic effect was most likely obtained due to melting of the test item. The second endothermic effect was probably obtained due to reaction and/or decomposition of the test item.

After the experiment, a dark yellow 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 endothermic effect, Experiment 2 was stopped directly after the melting effect. The extrapolated onset temperature was 156.165°C.

After the experiment, a colourless molten residue remained in the sample container (original colour: off-white). It demonstrated that melting was the reason for the endothermic effect. 

TGA and DSC curves: see illustration below.

 

RESULTS

Melting temperature: mean extrapolated onset temperature of DSC Experiment 1 (156.149°C) and Experiment 2 (156.165°C).

Boiling temperature: reaction and/or decomposition of the test item was observed during DSC experiment starting at 300°C. Boiling of the test item was not observed below the temperature at which reaction and/or decomposition started. Based on this, the test item has no boiling temperature.

 

Applicant's summary and conclusion

Conclusions:

The melting temperature of the substance was determined to be 156.2°C.

Executive summary:

Differential Scanning Calorimetry was performed. The experiments were in accordance with EC A.1, OECD 102 and OPPTS 830.7200 (melting temperature) and EC A.2, OECD TG 103 and OPPTS 830.722 (boiling temperature). GLP-study. 

The DSC curve showed an endothermic effect due to melting.

The melting temperature of the substance was determined in duplicate obtaining a mean value of 156.2°C.

 

Boiling of the substance was not observed below the temperature at which reaction and/or decomposition started (i.e. at 300°C). Based on this, the test item has no boiling temperature.