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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:
10 Mar - 03 May 2016
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Reason / purpose for cross-reference:
reference to other study
Reason / purpose for cross-reference:
reference to other 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), dry
Melting / freezing pt.:
ca. 154.1 °C
Atm. press.:
ca. 1 013 hPa
Decomposition:
yes
Decomp. temp.:
> 154.1 °C

Results
DSC measurement
Three measurements with a heating rate of 10 K/min showed an endothermal effect (melting) in the range of 140 to 170 °C. This was directly followed by an exothermal effect. The DSC measurements with a final temperature of 500 °C showed further endothermal and exothermal effects up to the final temperature. The onset temperature was derived from the intersection of the tangent line with the highest slope of the endothermal peak with the baseline.

An additional DSC measurement was done to determine whether melting was accompanied by decomposition. Therefore, the measurement was stopped at 162 °C. It showed an endothermal effect starting at 145 °C, no mass loss occurred.

Table 1 – Melting point – DSC measurement

Test item [mg]

Starting temperature [°C]

Final test temperature [°C]

Temperature range (melting) [°C]

Onset [°C]

Observations

6.91

25

500

140 – 165

154.26

Measurement was continued after melting

24.41

140 – 170

154.16

8.41

200

145 – 165

153.85

Test item was a solidified melt after the measurement, mass loss: 56%

16.97

162

Start: 145

-

Test item was a solidified melt after the measurement, no mass loss

 

Capillary tube in a metal block
To clarify the DSC results, a measurement with the capillary method was done.

Table 2 – Capillary method results

Set point [°C]

End point [°C]

Remarks

100

200

100 °C: test item appeared unchanged
Approx. 125 °C: test item started to melt
Approx. 163 °C: test item was completely molten
Approx. 165 °C: formation of bubbles, test item appears like white foam
Approx. 185 °C: test item rose in the capillary, appears like white foam

200 °C: no further changes

 

Conclusion: The test item had a melting point of 154.1 °C, afterwards decomposition started.

Description of key information

154.1 °C at 1013 hPa (OECD 102, DSC)

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:
154.1 °C

Additional information

Decomposition started directly after melting.