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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:
18 September 2012 - 17 December 2012
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Qualifier:
according to guideline
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
Version / remarks:
(2008)
Deviations:
no
Qualifier:
according to guideline
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Version / remarks:
(1995)
Deviations:
no
Qualifier:
according to guideline
Guideline:
EPA OPPTS 830.7200 (Melting Point / Melting Range)
Version / remarks:
(1998)
Deviations:
no
GLP compliance:
yes
Type of method:
differential scanning calorimetry
Key result
Melting / freezing pt.:
63 - 70 °C
Remarks on result:
other: Melting range 336-343 K

Preliminary TGA

From 100°C upwards the weight of the sample decreased significantly. At 169°C, the sample weight had decreased by 25%. The TGA curve shows a bend in the signal at approximately 150°C - 160°C indicating reaction/decomposition. After the experiment it was observed that the test sample had evaporated from the sample container.

 

DSC experiments

Experiment I: A first endothermic peak was observed between 25°C and 50°C (unknown effect). A second endothermic peak (probaly due to melting) was observed between 50°C and 100°C; the extrapolated onset temperature was 70.27°C. A third endothermic peak (probably due to reaction/decomposition) was observed between 100°C and 225°C. After the experiment the test substance had evaporated from the sample container.

 

Experiment II: To investigate the melting peak between 50°C and 100°C, a repeated heating cycle was applied. With the first heating, a first endothermic peak was observed between 25°C and 50°C and a second endothermic peak between 50°C and 100°C (extrapolated onset temperature: 63.00°C). During cooling, an exothermic (crystallization) peak was observed between 50°C and 65°C. A second exothermic effect was observed between 25°C and 40°C (unknown effect). With the second heating, a first endothermic peak was observed between 25°C and 50°C and a second endothermic peak between 50°C and 100°C (extrapolated onset temperature: 64.35°C). The results obtained confirmed that the second endothermic effect was due to melting. The endothermic peak between 100°C and 225°C had shifted to higher temperature (between 150°C and 250°C). After the experiment it was observed that the test sample had evaporated from the sample container.

 

Experiment III: Similar results as with Experiment I were obtained.The extrapolated onset of the melting peak was 69.95°C.

 

TGA/DSC curves: see attached document.

 

Conclusions:
The melting range of the substance was determined to be 63-70°C using differential scanning calorimetry in accordance with EC A.1, OECD 102 and EPA OPPTS 830.7200 and in compliance with GLP.

Description of key information

The melting range of the substance was determined to be 63-70°C (DSC: EC A.1, OECD 102 and EPA OPPTS 830.7200).  

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:
63 °C

Additional information

The lowest value of the range was taken as key value.