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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:
12-03.-26.06.2014
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Qualifier:
according to guideline
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
Deviations:
no
GLP compliance:
no
Type of method:
differential scanning calorimetry
Remarks:
and capillary method
Key result
Melting / freezing pt.:
> 61 - < 177 °C
Atm. press.:
1 013 hPa
Decomposition:
no
Sublimation:
no

Two DSC-measurements in aluminium crucibles with a hole showed three endothermic effects in the temperature range of 60 - 75 °C, 105 - 115 °C and 170 - 185 °C. The onset temperature is derived from the intersection of the tangent line with the highest slope of the endothermic peak with the baseline. The corresponding onset temperatures of the three endothermic effects are shown in table 1. No onset temperatures can be clearly assigned to a melting process.

Table 1: DSC measurements

ID

Onset/ °C

Temperature range/ °C

Crucible

34309

60.96

60 -75

Aluminium with a hole

108.05

105 - 115

176.94

170 - 185

34308

61.22

60 - 75

Aluminium with a hole

108.06

105 - 115

177.33

170 - 185

Additional measurements with the capillary method were performed in order to clarify the results of the DSC measurements.

Table 2: Capillary measurements

Set point/ °C

Heating rate/ K/min

End point/ °C

Phase change/ °C

Phase change/ °C

Phase change/ °C

30

10

150

67

111

-

30

10

150

67

111

-

30

10

150

68

111

-

60

1

68

64

-

-

50

10

210

67

109

179

In the temperature range of 30 - 64 °C the test item appeared as unchanged white crystals. In the temperature range of 64 - 67 °C the test item changed into cloudy I waxy and partly melted (phase change of the liquid crystal). Above 109 - 111 °C the test item changed into a cloudy liquid (phase change of the liquid crystal). Above 179 °C the test item changed into a clear liquid (phase change of the liquid crystal, clearing point). Due to the results of the DSC measurements and the capillary measurements it is concluded that the test item has a melting range of 61 - 177 °C with the occurrence of at least one mesophase.

Conclusions:
The test item has a melting range of 61 - 177 °C.
Executive summary:

A study was conducted according to OECD TG 102 and Regulation (EC) No 440/2008 method A.1 to determine the melting point of the test item using differential scanning calorimetry and capillary tube method.

Two DSC-measurements in aluminium crucibles with a hole showed three endothermic effects in the temperature range of 60 - 75 °C, 105 - 115 °C and 170 - 185 °C.

Additional measurements with the capillary method were performed in order to clarify the results of the DSC measurements.

In the temperature range of 30 - 64 °C the test item appeared as unchanged white crystals. In the temperature range of 64 - 67 °C the test item changed into cloudy I waxy and partly melted (phase change of the liquid crystal). Above 109 - 111 °C the test item changed into a cloudy liquid (phase change of the liquid crystal). Above 179 °C the test item changed into a clear liquid (phase change of the liquid crystal, clearing point). Due to the results of the DSC measurements and the capillary measurements it is concluded that the test item has a melting range of 61 - 177 °C with the occurrence of at least one mesophase.

Description of key information

The test item has a melting range of 61 - 177 °C

Key value for chemical safety assessment

Additional information

A study was conducted according to OECD TG 102 and Regulation (EC) No 440/2008 method A.1 to determine the melting point of the test item using differential scanning calorimetry and capillary tube method.

Two DSC-measurements in aluminium crucibles with a hole showed three endothermic effects in the temperature range of 60 - 75 °C, 105 - 115 °C and 170 - 185 °C.

Additional measurements with the capillary method were performed in order to clarify the results of the DSC measurements.

In the temperature range of 30 - 64 °C the test item appeared as unchanged white crystals. In the temperature range of 64 - 67 °C the test item changed into cloudy I waxy and partly melted (phase change of the liquid crystal). Above 109 - 111 °C the test item changed into a cloudy liquid (phase change of the liquid crystal). Above 179 °C the test item changed into a clear liquid (phase change of the liquid crystal, clearing point). Due to the results of the DSC measurements and the capillary measurements it is concluded that the test item has a melting range of 61 - 177 °C with the occurrence of at least one mesophase.

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