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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:
09.08.2016 - 13.12.2016
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Qualifier:
according to guideline
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
Deviations:
no
Qualifier:
according to guideline
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Deviations:
no
GLP compliance:
no
Type of method:
differential scanning calorimetry
Remarks:
and capillary method
Key result
Melting / freezing pt.:
219.3 °C
Atm. press.:
1 013.3 hPa
Decomposition:
no
Sublimation:
no

Melting point / melting range: DSC measurement

Two DSC measurements in aluminium crucibles with a hole with a heating rate of 10 K/min showed two endothermal effects (melting). The first endothermal effect occurred in the temperature range of 200 - 210 °C. The second endothermal effect occurred in the temperature range of 210 - 230 °C. A third endothermal effect was assigned to boiling.

Table 1: Melting point (DSC measurements)

Ident No.

Test item mg

Starting temperature °C

Final test temperature °C

Temperature range (melting) °C

Onset °C

Crucible

Observations after the measurement

35753

10.04

25

500

200 – 210

210 – 230

206.37

219.08

Aluminium with a hole

-

35754

14.95

25

500

205 – 210

210 – 230

206.61

219.46

Aluminium with a hole

-

 

An additional measurement with the capillary method was performed in order to clarify the melting point / range (two endothermal effects).

Melting point / melting range: capillary tube in a metal block

A measurement with the capillary method was performed to clarify the results of the DSC measurements. Since this measurement was performed only as a verifying screening a high heating rate of 10 K/min was chosen and, therefore, the absolute temperature values derived with the capillary method are not as accurate as the DSC results. The filling height of the test item was approximately 5 mm.

Table 2: Results of the capillary method

No.

Set point / °C

Heating rate / K/min

End point / °C

Remarks

1

160

10

250

(Test item is a white powder at ambient temperature)

Start at 160 °C: test item appeared unchanged

Approx. 211 °C: test item started to melt

Approx. 222 °C: test item was completely melted (clear)

End at 250 °C: no further changes

Under consideration of the results from the DSC measurements and the capillary method it was concluded that the test item melted at 219.3 °C.

Conclusions:
The melting point of the test substance was determined to be 219.3 °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 of the test item using differential scanning calorimetry. The test item was weighed into an aluminium crucible under an inert atmosphere (nitrogen). Two tests with 10 mg and 14 mg of the test item were performed. The crucible was heated from room temperature to 500 °C with 10 K/min heating rate. The two DSC measurements showed two endothermal effects (melting). The first endothermal effect occurred in the temperature range of 200 - 210 °C. The second endothermal effect occurred in the temperature range of 210 - 230 °C. A measurement with the capillary method was performed to clarify the results of the DSC measurements. A heating rate of 10 K/min was applied. The filling height of the test item was approximately 5 mm. At approximately 211 °C the test item started to melt and at 222 °C it was completely melted. Under consideration of the results from the DSC measurements and the capillary method it was concluded that the test item melted at 219.3 °C.

Description of key information

The melting point of the test substance was determined to be 219.3 °C.

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:
219.3 °C

Additional information

A study was conducted according to OECD TG 102 and Regulation (EC) No 440/2008 method A.1 to determine the melting point of the test item using differential scanning calorimetry. The test item was weighed into an aluminium crucible under an inert atmosphere (nitrogen). Two tests with 10 mg and 14 mg of the test item were performed. The crucible was heated from room temperature to 500 °C with 10 K/min heating rate. The two DSC measurements showed two endothermal effects (melting). The first endothermal effect occurred in the temperature range of 200 - 210 °C. The second endothermal effect occurred in the temperature range of 210 - 230 °C. A measurement with the capillary method was performed to clarify the results of the DSC measurements. A heating rate of 10 K/min was applied. The filling height of the test item was approximately 5 mm. At approximately 211 °C the test item started to melt and at 222 °C it was completely melted. Under consideration of the results from the DSC measurements and the capillary method it was concluded that the test item melted at 219.3 °C (reference 4.2-1).