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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:
19 July 2017 - 01 June 2018
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Remarks:
Study was conducted in accordance with international guidelines and in accordance with GLP. All guideline validity criteria were met.
Qualifier:
according to guideline
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
Version / remarks:
Regulation (EC) 440/2008 of 30 May 2008
Deviations:
no
Qualifier:
according to guideline
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Version / remarks:
27 July 1995
Deviations:
no
GLP compliance:
yes (incl. QA statement)
Type of method:
differential scanning calorimetry
Key result
Melting / freezing pt.:
>= 59.2 - <= 81 °C
Decomposition:
no
Sublimation:
no
Remarks on result:
other: Mean value

Evaluation of Data:

The melting/freezing point is defined as the point at which phase transition from solid to liquid state (or vice versa) at normal atmospheric pressure takes place. As the phase transition of many substances takes place over a large temperature range, it is often described as a melting/freezing range. During thermal analysis, the peak width of an endothermic reaction also depends on sample amount and heating rate. Therefore, the onset point of the relevant endothermic peak is usually stated as the freezing/melting point. If the endothermic peak/s is poorly defined, a range may be stated. Measured temperatures were converted from °C to K using Equation 1.

 

Equation 1:                                                                             

T = t + 273.15

where:

T = Thermodynamic temperature, Kelvin (K)

t = Celsius temperature, degrees Celsius (°C)

 

 

Results:

Table 2:          Thermographic Data – Preliminary Screen

Thermal Event

Interpretation

Temperature

Preliminary Test, Screen 1

Preliminary Test, Screen 2

°C

K

°C

K

Endotherm (onset)

Start of melting

67.2

340.2

66.6

339.8

The residue in the crucibles from the preliminary tests was observed to be dark brown staining around the periphery of the crucible most likely due to decomposition.

 

 

Table 3:          Thermographic Data – Preliminary Screen

Thermal Event

Interpretation

Temperature

Main Test, Determination 1

Main Test, Determination 2

°C

K

°C

K

Endotherm (lower limit)

Start of melting

59.6

332.8

58.9

332.1

Endotherm (upper limit)

End of melting

80.9

354.1

81.0

354.2

 

Conclusion:

The melting point of the test item has been determined to be in the range of 59.2 to 81.0 °C (332.8 to 354.0 K).

Conclusions:
The test item has a mean melting point of 59.2 - 81.0 °C ± 0.5 °C (332.35 - 354.15 K ± 0.5 K).
Executive summary:

EU Method A.1. – The melting point/freezing point of the test item was determined using the Differential Scanning Calorimeter (DSC) method.  The procedure employed was designed to be compatible with Method A.1. Melting/Freezing Temperature of Commission Regulation (EC) No 440/2008 of 30 May 2008.

Aliquots of test item (0.0053 – 0.0058 mm) were placed in a crucible and subjected to heating at a rate of 1 °C/min from 25 to 110 °C.  Heating was continued until melting of the sample was observed.  The main test was performed two times.

The mean melting temperature of the test item was determined to be 59.2 - 81.0 °C ± 0.5 °C.

Description of key information

Melting Point: 59.2 - 81.0 °C ± 0.5 °C (332.35 - 354.15 K ± 0.5 K); EU Method A.1.; R. Butler (2018)

Key value for chemical safety assessment

Additional information

EU Method A.1. – The melting point/freezing point of the test item was determined using the Differential Scanning Calorimeter (DSC) method.  The procedure employed was designed to be compatible with Method A.1. Melting/Freezing Temperature of Commission Regulation (EC) No 440/2008 of 30 May 2008.

Aliquots of test item (0.0053 – 0.0058 mm) were placed in a crucible and subjected to heating at a rate of 1 °C/min from 25 to 110 °C.  Heating was continued until melting of the sample was observed.  The main test was performed two times.

The mean melting temperature of the test item was determined to be 59.2 - 81.0 °C ± 0.5 °C.