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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:
20 to 21 April 2016
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Reason / purpose for cross-reference:
reference to same study
Qualifier:
according to guideline
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
Qualifier:
according to guideline
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Qualifier:
according to guideline
Guideline:
EPA OPPTS 830.7200 (Melting Point / Melting Range)
Qualifier:
according to guideline
Guideline:
other: CIPAC MT 1 (2009): Freezing Point
GLP compliance:
no
Type of method:
differential scanning calorimetry
Key result
Melting / freezing pt.:
-53 °C
Atm. press.:
1 017 hPa
Decomposition:
no

Results

In the temperature range of -60 to -40 °C, a very small endothermic effect (melting) was observed. Between approx. 180 - 320 °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

PN10910

19.32

-53.25

293.55

-60 to -40 (endo)

190 - 320 (endo)

19.28

1017.2

PN10911

17.70

-53.49

292.90

-60 to -40 (endo)

180 - 320 (endo)

17.53

1017.2

 

During the cooling phase, no thermal effects were observed, which can be associated with the freezing of the test item.

During the heating phase a very small endothermic effect was observed in the temperature range of -60 to -40 °C, which can be assigned to the melting of the test item. As the onset temperatures in both tests deviate by less than 0.5 K from their mean value of -53.37 °C, the test item has a melting point of -53 °C.

Due to the low energy of the melting peak, the melting of the test item was verified. 5.6 g of the test item in a test tube were cooled down with liquid nitrogen to approx. -65 °C. At this temperature the test item was solid. The appearance of the test item during warming up: between -52 to -45 °C very viscous, at -40 °C liquid. Therefore the melting point in the DSC-measurement was confirmed.

The test item showed a second endothermic signal in the temperature range of approx. 180 - 320 °C that can be assigned to the boiling of the test item.

No further thermal effects were observed up to the maximum test temperature of 500 °C.

 

Final Results

The test item has a melting point of -53 °C at atmospheric pressure (1017 hPa) as determined by differential scanning calorimetry according to Regulation EC No. 440/2008 Method A.1. and OECD Test Guideline 102 (1995).

Conclusions:
A melting point of -53 °C (at 1017 hPa) was determined for the test substance according to EU Method A.1

Description of key information

Melting point: -53 °C at 1017 hPa (EU Method A.1, differential scanning calorimetry)

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:
-53 °C

Additional information

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