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Melting point / freezing point

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Endpoint:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
key study
Study period:
Not reported
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Qualifier:
according to
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
Deviations:
not specified
GLP compliance:
not specified
Type of method:
differential scanning calorimetry
Melting / freezing pt.:
>= 177.59 - <= 178.07 °C
Remarks on result:
other: 1st endothermic effect (°C)
Melting / freezing pt.:
>= 204.39 - <= 204.58 °C
Remarks on result:
other: 2nd endothermic effect (°C)
Melting / freezing pt.:
>= 231.97 - <= 232.76 °C
Remarks on result:
other: 3rd endothermic effect (°C)

After the experiment the color of the sample was dark brown.

The means of the two measurements of the 1st and 2nd endothermic effect are in the range of the estimated accuracy given by the method in Regulation (EC) No 440/2008, A.1 therefore they are reported as the melting temperature. The mean of the two measurements of the 3rd endothermic effect is not in the range of the estimated accuracy given by the method in Regulation (EC) No 440/2008, A.1 therefore two temperatures are reported.

The fourth endothermic heat effect might correspond to the boiling point and/or decomposition temperature of the test item. The reference material melts at 327,50 °C, thus confirming the performance of the test method.

Table 1: Test item melting point results

   Heating Range  Heating Rate (°C/min)  1st endothermic effect (°C)   2nd endothermic effect (°C)  3rd endothermic effect (°C)    4th endothermic effect (°C)
 1st Test  25 °C to 390 °C  10  178.07  204.58  231.97  292.42
 2nd Test

 25 °C to 390 °C

 10  177.59  204.39  232.76  293.19
Conclusions:
Melting of the test item begins at 177.8 °C. The test item is a UVCB substance thus a range of melting is detected. The second melting point is 204.5 °C and the third melting point is in the range 232.0 – 232.8 °C.
Executive summary:

The melting point of the test item was determined in an EC A.1 guideline study using the differential scanning calorimeter method. The test item was tested in duplicate, and lead was also tested as a reference item. The test item is a UVCB and therefore, a range of melting points were determined. Melting of the test item begins at 177.8 °C, the second melting point is 204.5 °C and the third melting point is in the range 232.0 – 232.8 °C. A fourth endothermic effect was also observed and it was determined that this might correspond to the boiling point and/or decomposition temperature of the test item. The reference material melted at 327.50 °C, thus confirming the performance of the test method.

The study is a guideline experimental study and is determined to be adequate for assessment of this endpoint without restrictions.

Endpoint:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
key study
Study period:
07 July 2017
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Qualifier:
according to
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Qualifier:
according to
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
GLP compliance:
yes (incl. certificate)
Type of method:
capillary method
Remarks:
Metal block method
Key result
Decomposition:
yes
Decomp. temp.:
>= 174 °C
Remarks on result:
other: Test item decomposed without melting
Remarks:
the samples were observed to darken at temperatures above approximately 174 °C, indicating decomposition.
Conclusions:
The melting temperature of the test item was not determinable as the test item decomposed at temperatures above approximately 174 °C without melting.
Executive summary:

The melting temperature of the test item was investigated in a study performed according to OECD 102 and EC Method A.1. guidelines. The melting temperature of the test item was not determinable as the test item decomposed at temperatures above approximately 174 °C without melting.

The study is a GLP compliant, guideline experimental study, and is acceptable without restrictions.

Description of key information

The melting point of the test item was determined in two guideline studies. In the study Cage (2018) the melting point was not determinable as the substance decomposed at temperatures above approximately 174 °C without melting. In the study Puke (2009) melting of the test item began at 177.8 °C, the second melting point was at 204.5 °C and the third melting point in the range 232.0 – 232.8 °C. After the experiment the colour of the sample was dark brown.

Key value for chemical safety assessment

Additional information

In the study Cage (2018) the melting temperature of the test item was investigated in a study performed according to OECD 102 and EC Method A.1. and GLP guidelines. In the study Puke (2009) the melting point of the test item was determined in an EC A.1 guideline study using the differential scanning calorimeter method.

Both studies followed standard test guidelines and are considered reliable without restrictions.