(1R,4S,4aR,8aS)-9-(dichloromethylidene)octahydro-1,4-methanonaphthalene-5,8-dione

Melting point / freezing point

Link to relevant study record(s)

Reference

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

2011-02-04 (experimental phase)

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

other: The study was conducted according to a relevant guideline without deviations. It was not carried out according to GLP, but it was performed in a test facility which has been certified to be in compliance with the principles of GLP.

Qualifier:

according to guideline

Guideline:

EU Method A.1 (Melting / Freezing Temperature)

Version / remarks:

from May 30, 2008

Deviations:

no

Qualifier:

according to guideline

Guideline:

OECD Guideline 102 (Melting point / Melting Range)

Version / remarks:

adopted July 27, 1995

Deviations:

no

GLP compliance:

no

Remarks:

However, the study was performed in a test facility which has been certified to be in compliance with the principles of GLP.

Type of method:

thermal analysis

Melting / freezing pt.:

175.5 °C

Atm. press.:

ca. 1 atm

Decomposition:

no

Sublimation:

no

Remarks on result:

other: Atmospheric pressure is not reported, however it is assumed that the test was performed at ambient pressure.

Preliminary Test

An endothermic heat effect was observed starting at 177.8 °C. After the experiment, the sample had lost about 61% of its mass and a black carbonized foam residue remained.

Main Tests

In order to determine the melting more precisely, further differential scanning calorimetry-runs were recorded between 120 °C and 220 °C with a heating rate of 10 °C/min. In the first main test run, the melting was observed at 175.3 °C, during the second main test run at 175.7 °C. During these runs, the samples lost about 3% of their mass and a brown melt remained in the sample cups.

Determination of the Melting Point

	Heating Range [°C]	Heating Rate [°C/min]	Melting Point [°C]	Melting Point [K]
Preliminary Test	25 - 400	20	177.8	451.0
1^stMain Test	120 - 220	10	175.3	448.5
2^ndMain Test	120 – 220	10	175.7	448.9
Mean of melting point*:			175.5	448.7

 *The mean melting point was calculated from the two results of the Main Tests (onset point of the endothermic reaction).

 

Conclusions:

The melting point of the test item was determined to be 175.5 ± 0.5 °C. The study is considered to be adequate and reliable.

Executive summary:

The determination of the melting point/melting range of the test item was performed according to the OECD Guideline No. 102: “Melting point / melting range“, adopted July 27, 1995 by thermal analysis.

In a preliminary test done by differential scanning calorimetry, an endothermic heat effect was observed starting at 177.8 °C. In order to determine the melting more precisely, further differential scanning calorimetry-runs were recorded between 120 °C and 220 °C with a heating rate of 10 °C/min during the main test. In the first main test run, the melting was observed at 175.3 °C, during the second main test run at 175.7 °C.

The melting point of the test item was determined to be 175.5 ± 0.5 °C.

 

 

Description of key information

175.5 ± 0.5 °C,  OECD 102, DSC; thermal analysis, Kühne 2011. 

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:

175.5 °C

Additional information

Only a single study conducted according to guidelines is available for this endpoint. The study is considered to be relevant, reliable (Klimisch 1) and adequate for the purposes of risk assessment, classification and labelling.