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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:
16/03/16, 05/05/2016 and 24/05/2016
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Qualifier:
according to guideline
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
GLP compliance:
no
Other quality assurance:
other: ISO9001-2008
Remarks:
TECNIO network
Type of method:
differential scanning calorimetry
Key result
Decomposition:
yes
Decomp. temp.:
187 °C
Remarks on result:
not determinable
Remarks:
the substance decomposes before melting

 Differential Scanning Calorimetry (DSC) High-Pressure Diferential Scanning Calorimetry (DSC-HP) Thermogravimetric analysis (TGA): 
 Equipment  Mettler Toledo DSC-822e   Mettler Toledo DSC-822e  Mettler Toledo TGA/SDTA851e
 Crucible  Aluminium crucible with a capacity of 40 microL.  gold plated high pressure crucible with a capacity of 30 microL (hermetically sealed until 150 bar)  Alumina crucible with a capacity of 70 microL.
 Gas  dry nitrogen at 50mL/min  dry nitrogen at 50 mL/min  Dry nitrogen 50 mL/min.
 Method  Heating from 30ºC to 600ºC at a rate of 10ºC/min   Heating from 30ºC to 400ºC at a rate of 10ºC/min

 Heating from 30°C to 600°C at a rate of l0ºC/min. Previously, a blank curve has

been performed and it has been subtracted.

Conclusions:
The substance decomposes at 187ºC without melting
Executive summary:

A first DSC has been done and the sample has shown an endothermic phenomenon starting at 187ºC with an associated heat of 330.6 J/g

In view of these results, the same sample has been analysed by DSC-HP (in inert atmosphere, nitrogen) showing an exothermic phenomenon from 197°C with a peak at 208°C and an associated heat of 362.9 J/g which could be attributed to the thermal decomposition of the sample.

The sample sample has been by TGA showing a first weight loss of 7.9% from 30°C to 224°C, a second weight loss of 8.9% from 224°C to 278°C and a third weight loss of 32.5% from 280°C to 598°C.

Description of key information

The determination has been done using DSC and DSC-HP (inert atmosphere with nitrogen) techniques.

The substance decomposes at 187ºC without melting.

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:
300 °C

Additional information

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