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Melting point / freezing point

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Reference
Endpoint:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
key study
Study period:
2018-11-20 to 2019-01-17
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Qualifier:
according to guideline
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Deviations:
no
Qualifier:
according to guideline
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
Deviations:
no
GLP compliance:
yes (incl. QA statement)
Type of method:
differential scanning calorimetry
Key result
Melting / freezing pt.:
80 - 82 °C
Atm. press.:
1 013.25 hPa
Decomposition:
no
Sublimation:
no

Results of the DSC-measurements

During the heating phase a distinct endothermic effect was observed in the temperature range of 70 – 100 °C, which was assigned to the melting of the test item.

 

Results of the DSC measurements

Sample
weight /
mg

Onset of
effect / °C

Range of effect

/°C

Weight
loss/
mg

Atmospheric
pressure/
hPa

14.53

80.17
222.49

70- 100 (endo)
160 -240 (endo)

14.53

1007.9

15.77

82.03
221.92

70- 100 (endo)
160 -240 (endo)

15.77

990.8

 

Capillary Method

For verification of the result for the melting temperature, the test item was additionally tested according to the capillary method. The test item was homogenised prior to the test by pounding with a mortar and pestle. In the three tests, the test item melted at an average temperature of 81.0 °C.

As the onset temperatures from both test runs deviate by more than 0.5 K from their mean value of 81.10 °C, a melting range of 80 – 82 °C was given instead of a melting point.

Conclusions:
The melting range of the test item was determined to be from 80 to 82 °C.
Executive summary:

A study was conducted according to OECD test guideline 102, Regulation (EC) No 440/2008 method A.1 and EPA OCSPP test guideline 830.7200 to determine the melting point of the test item using differential scanning calorimetry. The test item was weighed out into an aluminium crucible under an inert atmosphere (nitrogen). Two tests with about 14 – 16 mg of the test item were performed. As reference crucible, an empty aluminium crucible was used. Under ambient conditions, the test item is solid. Therefore, the tests were started at ambient temperature. During the heating phase a distinct endothermic effect was observed in the temperature range of 70 – 100 °C, which was assigned to the melting of the test item. As the onset temperatures from both test runs deviate by more than 0.5 K from their mean value of 81.1 °C, a melting range of 80 – 82 °C was given instead of a melting point. For verification of the result for the melting temperature the test item was additionally tested according to the capillary method. The test item was homogenised prior to the test by pounding with a mortar and pestle. In the three tests, the test item melted at an average temperature of 81.0 °C. Thus, the melting range of the test item was determined to be from 80 to 82 °C.

Description of key information

The melting range of the test item was determined to be from 80 to 82 °C (reference 4.2 -1).

Key value for chemical safety assessment

Additional information

A study was conducted according to OECD test guideline 102, Regulation (EC) No 440/2008 method A.1 and EPA OCSPP test guideline 830.7200 to determine the melting point of the test item using differential scanning calorimetry (reference 4.2 -1). The test item was weighed out into an aluminium crucible under an inert atmosphere (nitrogen). Two tests with about 14 – 16 mg of the test item were performed. As reference crucible, an empty aluminium crucible was used. Under ambient conditions, the test item is solid. Therefore, the tests were started at ambient temperature. During the heating phase a distinct endothermic effect was observed in the temperature range of 70 – 100 °C, which was assigned to the melting of the test item. As the onset temperatures from both test runs deviate by more than 0.5 K from their mean value of 81.10 °C, a melting range of 80 – 82 °C was given instead of a melting point. For verification of the result for the melting temperature the test item was additionally tested according to the capillary method. The test item was homogenised prior to the test by pounding with a mortar and pestle. In the three tests, the test item melted at an average temperature of 81.0 °C. Thus, the melting range of the test item was determined to be in range from 80 to 82 °C.