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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:
23 Jul - 11 Aug 2015
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
other:
Reason / purpose for cross-reference:
reference to same study
Reason / purpose for cross-reference:
reference to same study
Qualifier:
according to guideline
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Qualifier:
according to guideline
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
GLP compliance:
no
Type of method:
differential scanning calorimetry
Specific details on test material used for the study:
Storage conditions: ambient temperature (10 – 30 °C)
Melting / freezing pt.:
ca. 231.8 °C
Atm. press.:
ca. 1 013 hPa
Remarks on result:
other: The capillary method measurement showed that the test item melted in a temperature range of 218°C to 238°C.

Results
DSC
Two DSC measurements showed two endothermal effects in the ranges 95 – 115 °C and 215 – 235 °C. The second endothermal effect was directly followed by an exothermal effect. Because of this, an additional measurement with the capillary method was done.

Due to the result from the capillary measurement, additional DSC measurements were done to exclude the influence of the crucible material on the results. Only these measurements in glass crucibles with a heating rate of 10 K/min were used for the final evaluation.

Two endothermal effects were seen in the ranges of 100 – 125 °C and 225 – 255 °C, before boiling. Based on results from the capillary melting, it was concluded that the test item melted during the second endothermal effect, it had a melting point of 231.8 °C.

Table 1- Melting point (DSC)

Test item [mg]

Starting temperature [°C]

Final test temperature [°C]

Temperature range (melting) [°C]

Onset [°C]

Crucible

Observations

12.60

25

500

95 – 115
215 – 235

Ambiguous

Aluminium with a hole

Crucible was empty after measurement

9.43

95 – 110
220 – 235

13.46

100 – 125
225 – 250

n.r.
231.5

Glass, open

Measurement continued after melting

20.25

100 – 125
225 - 255

n.r.
232.0

n.r. not relevant

Melting Point: Capillary tube in a metal block
Table 2 - Results

Set point [°C]

Heating rate [K/min]

End point [°C]

Remarks

80

10

400

Approx. 94 °C: test item appeared glassy
Approx. 218 °C: test item started to melt
Approx. 238 °C: test item fully melted

Approx. 101 °C: test item appeared glassy
Approx. 221 °C: test item started to melt
Approx. 237 °C: test item fully melted

 

The capillary method showed that the test item melted in the temperature range of 218 – 238 °C.

Conclusion: The test item has a mean melting point of 231.8 °C.

Description of key information

231.8 °C at 1013 hPa (OECD 102, DSC)

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:
231.8 °C

Additional information