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Physical & Chemical properties

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:
from 2017-03-23 to 2017-06-12
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:
no
Type of method:
differential scanning calorimetry
Key result
Melting / freezing pt.:
< -20 °C

In the first measurement the test item was cooled down from 25 °C to -50 °C with a cooling rate of 10 K/min. After -50 °C had been reached, the sample was kept at this temperature for 60 min. Afterwards, it was heated up from -50 °C to 500 °C at a constant heating rate of 10 K/min. The DSC measurement in an aluminium crucible with a hole showed no exothermal effect (crystallisation) in the cooling-down phase. The measurement showed no significant endothermal effect (melting) in the heating-up phase until an ambient temperature was reached. However, around -40 °C a small endothermal effect could be detected.

In the second measurement the test item was cooled down from 25 °C to -80 °C with a cooling rate of 3 K/min. After -80 °C had been reached, the sample was kept at this temperature for 60 min. Afterwards, the test item was heated up from -80 °C to 20 °C at a constant heating rate of 10 K/min. No exothermal effect (crystallisation) in the cooling-down phase and in the isothermal phase and no significant endothermal effect (melting) in the heating-up phase were observed. However, around -40 °C a small endothermal effect could be detected.

Table 1: Melting point (DSC measurements)

Test item / mg

Starting temperature / °C

Final test temperature / °C

Temperature range (endothermal) / °C

Onset (melting) / °C

Crucible

Observations after the measurement

13.29

25

-50 / 500

-

-

Aluminium with a hole

-

12.12

25

-80 / 20

-

-

Aluminium with a hole

-

No melting point was measured above -100 °C. However, since melting may be hindered at low temperatures due to supercooling and due to a small endothermal effect of unknown origin around -40 °C it can only be assumed that no melting point exists above -20 °C.

Conclusions:
No melting point could be determined for the test item above -100 °C. Therefore, the freeing point of the test item is <-20 °C.
Executive summary:

A study was conducted according to OECD TG 102 and Regulation (EC) No 440/2008 method A.1 to determine the melting point/range of the test item using differential scanning calorimetry. The test item was weighed into an aluminium crucible under an inert atmosphere (nitrogen). Two measurements with about 12 – 13 mg of the test item were performed. As reference crucible, an empty aluminium crucible was used. The crucible was cooled down from 25 °C to -50 °C with 10 K/min cooling rate. It was kept at this temperature for 60 min and then heated up to 500 °C with a constant heating rate of 10 K/min. No endothermal and exothermal effects were observed. In a second measurement the crucible was cooled down from 25 °C to -80 °C with a cooling rate of 3 K/min. It was kept at -80 °C for 60 min and then heated up to 20 °C with a constant heating rate of 10 K/min. Again no exothermal and endothermal effects were observed. At around -40 °C a small endothermal effects was observed in both measurements. No melting point could be determined to -100 °C. Therefore, the freezing point of the test item is <-20 °C.

Description of key information

No melting point could be determined for the test item above -100 °C. Therefore, the freezing point of the test item is <-20 °C.

Key value for chemical safety assessment

Additional information

A study (reference 4.2-1) was conducted according to OECD TG 102 and Regulation (EC) No 440/2008 method A.1 to determine the melting point/range of the test item using differential scanning calorimetry. The test item was weighed into an aluminium crucible under an inert atmosphere (nitrogen). Two measurements with about 12 – 13 mg of the test item were performed. As reference crucible, an empty aluminium crucible was used. The crucible was cooled down from 25 °C to -50 °C with 10 K/min cooling rate. It was kept at this temperature for 60 min and then heated up to 500 °C with a constant heating rate of 10 K/min. No endothermal and exothermal effects were observed. In a second measurement the crucible was cooled down from 25 °C to -80 °C with a cooling rate of 3 K/min. It was kept at -80 °C for 60 min and then heated up to 20 °C with a constant heating rate of 10 K/min. Again no exothermal and endothermal effects were observed. At around -40 °C a small endothermal effect was observed in both measurements. No melting point could be determined to -100 °C. Therefore, the freezing point of the test item is <-20 °C.