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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:
2018-03-27 to 2018-07-30
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Qualifier:
according to
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Version / remarks:
1995
Deviations:
no
Qualifier:
according to
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
Version / remarks:
2008
Deviations:
no
GLP compliance:
yes (incl. certificate)
Type of method:
differential scanning calorimetry
Key result
Melting / freezing pt.:
229.4 °C
Decomposition:
yes
Decomp. temp.:
220 °C

Results

In the temperature range of 220 - 250 °C, 250 - 280 °C and 290 - 320 °C three endothermic effects were observed. In the temperature range of 320 - 370 °C an exothermic effect was observed, with a decomposition energy of approx. -40 J/g.

Table 1: Results of DSC-measurements

No.

Sample

Onset of Effect/ °C

Range of effect/ °C

Weight loss/ mg

Atmospheric presure/ hPa

PN15597

10.76

229.13

260.03

310.84

220 – 250 (endo)

250 – 280 (endo)

290 – 320 (endo)

320 – 360 (exo)

5.27

1007.4

PN15598

10.91

229.62

257.10

307.42

220 – 250 (endo)

250 – 280 (endo)

290 – 320 (endo)

320 – 370 (exo)

4.48

1007.4

During the heating phase three endothermic effects were observed, which can't be clearly assigned to a melting of the test item. Thus, the capillary method was performed for a verification of the DSC-measurements.

Three capillaries were filled with the test item up to a height of 4 - 6 mm. The capillaries were heated up from 30 to 200 °C with a constant heating rate of 10 K/min and from 200 to 400 °C with a constant heating rate of 10 K/min in the BÜCHI melting point apparatus. The test item was visually observed while increasing the temperature.

The melting of the test item could be observed at approx. 212 °C. The test item darkened at approx. 220 °C and its colour changed to black at approx. 280 °C. No boiling of the test item could be observed up to the decomposition of the test item.

Combining the results of the measurements, the first endothermic effect in the DSC in the temperature range of 220 to 250 °C can be assigned to a melting of the test item. As the onset temperatures in both tests do not deviate by more than 0.5 K from their mean value of 229.4 °C, the test item has a melting point of 229.4 °C under decomposition, which starts at approx. 220 °C.

No boiling of the test item could be observed up to the decomposition, starting at approx. 220 °C.

Conclusions:
The test substance has a melting point of 229.4 °C under decomposition at atmospheric pressure (1007 hPa).
Executive summary:

The test substance has a melting point of 229.4 °C under decomposition at atmospheric pressure (1007 hPa) as determined by differential scanning calorimetry and confirmed by the capillary method according to Regulation Ec No. 440/2008 Method A.1. and OECD Guideline 102 (1995).

Description of key information

The test substance has a melting point of 229.4 °C under decomposition at atmospheric pressure (1007 hPa).

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:
229.4 °C

Additional information

The test substance has a melting point of 229.4 °C under decomposition at atmospheric pressure (1007 hPa) as determined by differential scanning calorimetry and confirmed by the capillary method according to Regulation EC No. 440/2008 Method A.1. and OECD Guideline 102 (1995).