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Melting point / freezing point

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Endpoint:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
key study
Study period:
26-Aug-2014 to 27-Aug-2014
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Reason / purpose:
reference to same study
Qualifier:
according to
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
Qualifier:
according to
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Qualifier:
according to
Guideline:
EPA OPPTS 830.7200 (Melting Point / Melting Range)
GLP compliance:
no
Type of method:
thermal analysis
Remarks:
Differential scanning calorimetry (DSC)
Key result
Melting / freezing pt.:
-56.2 °C
Atm. press.:
1 013 hPa

Results

In the thermograms of the two DSC runs (nos. PN7356 and PN7368) an endothermic (melting) effect was observed in the temperature range of -60 °C to -45 °C. Between 100 to 265 °C a second endothermic effect (boiling) could be detected.

 

Results of the DSC measurements

No.

Sample weight (mg)

Onset of effect (°C)

Range of effect (°C)

Weight loss (mg)

Atmospheric pressure (hPa)

PN7356

10.43

-56.19

245.90

-60 to -45 (endo)

100 to 265 (endo)

10.43

993.8

PN7368

12.85

-56.10

246.19

-60 to -45 (endo)

130 to 260 (endo)

11.80

1004.2

 

The first endothermic effect was observed in the temperature range of -60 to -45 °C, which can be associated with the melting of the test item. As the onset temperatures in both tests do not deviate by more than 0.5 K from their mean value of -56.15 °C, this temperature can be used as the melting point. The test item has a melting point of -56.2 °C.

Final Results

The test item has a melting point of -56.2 °C at atmospheric pressure (1013 hPa) as determined by differential scanning calorimetry according to Directive EC440/2008 Method A.1., OECD Test Guideline 102 (1995), EPA OCSPP 830.7200 (1998) and CIPAC MT 1 (2009).

At ambient conditions, the test item is a liquid. Therefore the crucibles were cooled down from ambient temperature to -100 °C with a constant cooling rate of 0.25 K/min under an inert atmosphere. After a waiting period of 30 min at -100 °C, the temperature was increased up to 500 °C at a constant heating rate of 10 K/min.

Conclusions:
A melting point value of -56.2 °C (at 1013 hPa) was determined for the tst substance according to E.U. Method A.1.
Endpoint:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
key study
Study period:
06-Mar-2015
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Reason / purpose:
reference to same study
Qualifier:
according to
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
Qualifier:
according to
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Qualifier:
according to
Guideline:
EPA OPPTS 830.7200 (Melting Point / Melting Range)
GLP compliance:
no
Type of method:
thermal analysis
Remarks:
Differential scanning calorimetry (DSC)
Melting / freezing pt.:
-55.9 °C
Atm. press.:
1 024 hPa

Results

In the thermograms of the two DSC runs (nos. PN8424 and PN8425) an endothermic (melting) effect was observed in the temperature range of -60 °C to -50 °C. Between 100 to 260 °C a second endothermic effect (boiling) could be detected.

Results of the DSC measurements

No.

Sample weight (mg)

Onset of effect (°C)

Range of effect (°C)

Weight loss (mg)

Atmospheric pressure (hPa)

PN8424

11.42

-55.86

243.75

-60 to -50 (endo)

110 to 260 (endo)

11.42

1024.2

PN8425

10.43

-55.95

243.69

-60 to -50 (endo)

100 to 260 (endo)

10.43

1024.2

 

During the cooling phase no thermal effect was detected. During the heating phase an endothermic effect was observed in the temperature range of -60 to -50 °C, which can be associated with the melting of the test item. As the onset temperatures in both tests do not deviate by more than 0.5 K from their mean value of -55.91 °C, this temperature can be used as the melting point. The test item has a melting point of -55.9 °C.

Final Results

The test item has a melting point of -55.9 °C at atmospheric pressure (1024 hPa) as determined by differential scanning calorimetry according to Directive EC440/2008 Method A.1., OECD Test Guideline 102 (1995), EPA OCSPP 830.7200 (1998) and CIPAC MT 1 (2009).

Conclusions:
A melting point value of -55.9 °C (at 1013 hPa) was determined for the test substance according to E.U. Method A.1.

Description of key information

Melting point

Composition A: -56.2 °C at 1013 hPa (EU Method A.1, differential scanning calorimetry)

Composition B: -55.9 °C at 1013 hPa (EU Method A.1, differential scanning calorimetry)

Key value for chemical safety assessment

Additional information