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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:
From December 12 to August 03, 2018
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
test procedure in accordance with generally accepted scientific standards and described in sufficient detail
Qualifier:
according to guideline
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Version / remarks:
1995
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
Remarks:
and capillary method
Decomposition:
yes
Decomp. temp.:
ca. 240 °C

The item shows no melting until the decomposition starting at a temperature of approx. 240 °C.

DSC ANALYSIS

During the DSC analysis, a broad endothermic effect was observed in the temperature range of 50 – 240 °C, followed by two exothermic effects in the temperature range of 240 °C – 300 °C and 330 °C – 400 °C, respectively.

Replicate Sample weight / mg Onset of Effect / °C Range of effect / °C Energy / J/g Weight loss / mg
1 13.92 58.9 50 – 210 (endo) 112.14 3.05
--- 240 – 300 (exo) -17.38
--- 340 – 390 (exo) -7.91
2 16 79.7 70 – 240 (endo) 108.51 3.71
--- 240 – 300 (exo) -11.37
--- 330 – 400 (exo) -19.19

During the heating phase the test item showed no distinct endothermic signal, witch can be assumed with a melting point. The broad endothermic effect starting at approx. 50 °C was caused by another endothermic process (e.g. drying, gas evolution, boiling).

CAPILLARY METHOD

The capillary analysis confirmed that the test item showed no melting in the temperature range from ambient temperature to 400 °C; above 240 °C the colour of the test item became darker and at 400 °C the test item was grey.

Conclusions:
The item shows no melting until the decomposition starting at a temperature of approx. 240 °C.
Executive summary:

The thermal behaviour of test item was assessed using the DSC analysis, according to the OECD guideline 102; the temperature of the DSC apparatus was increased up to 500 °C at a constant heating rate of 10 K/min under air.

To verify the results of the DSC measurements, three additional measurements with the capillary method were performed in the temperature range of 25 – 400 °C with a heating rate of 10 K/min.

During the DSC analysis, a broad endothermic effect was observed in the temperature range of 50 °C – 240 °C, followed by two exothermic effects in the temperature range of 240 °C – 300 °C and 330 °C – 400 °C, respectively. During the heating phase the test item showed no distinct endothermic signal, which can be assumed with a melting point. The broad endothermic effect starting at approx. 50 °C was caused by another endothermic process (e.g. drying, gas evolution, boiling).

The capillary analysis confirmed that the test item showed no melting in the temperature range from ambient temperature to 400 °C; above 240 °C the colour of the test item became darker and at 400 °C the test item was grey.

Conclusion

The item shows no melting until the decomposition starting at a temperature of approx. 240 °C.

Description of key information

Decomposition before melting/boiling, starting at approx. 240 °C.

Key value for chemical safety assessment

Additional information

OECD 102 - differential scanning calorimetry and capillary methods

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