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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:
March 15, 2018
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.:
211.3 °C
Decomposition:
yes
Decomp. temp.:
> 215 °C

Melting point / melting range: DSC measurement

Two DSC measurements with a heating rate of 10 K/min showed an endothermal effect (melting) in the temperature range of 205 – 215 °C, followed by an exothermal effect in the temperature range 215 – 280 °C. The onset temperature (see Table1) was derived from the intersection of the tangent line with the highest slope of the endothermal peak with the baseline. In the first measurement a mass loss of 61 % occurred and a black residue was obtained after the measurement. The second measurement was terminated shortly after the beginning of the exothermal peak. Here a mass loss of only 4 % was determined and the test item was a solidified, black melt after the measurement.

The results of the DSC measurements are summarized in Table 1.

Table1: Melting point (DSC measurements)

Ident No.

Test item /

mg

Starting temperature /

°C

Final test temperature /

°C

Temperature range (endo-thermal) /

°C

Onset (melting) / °C

Crucible

Observations after the measurement

36874

9.14

25

500

205 – 215

211.04

Aluminium with a hole

Black residue, 61 % mass loss

36876

8.55

25

220

205 – 215

211.60

Aluminium with a hole

Test item was a solidified, black melt, 4 % mass loss

Due to the different mass losses in the first and second measurement and the observation of a solidified black melt in the second measurement, the melting point was determined to 211.3 °C. The melting point is directly followed by decomposition, starting at approx. 215 °C.

Executive summary:

The test item had a mean melting point of 211.3 °C.

Description of key information

The test item had a mean melting point of 211.3 °C.

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:
211.3 °C

Additional information