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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:
21 April 2017 - 13 November 2017
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:
EU Method A.1 (Melting / Freezing Temperature)
Version / remarks:
Regulation (EC) 440/2008 of 30 May 2008
Deviations:
no
Qualifier:
according to
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Version / remarks:
27 July 1995.
Deviations:
no
Qualifier:
equivalent or similar to
Guideline:
EPA OPPTS 830.7200 (Melting Point / Melting Range)
Version / remarks:
March 1998
Deviations:
not specified
Qualifier:
equivalent or similar to
Guideline:
other: CIPAC MT 1
Version / remarks:
2009
Deviations:
not specified
GLP compliance:
yes (incl. certificate)
Type of method:
differential scanning calorimetry
Key result
Melting / freezing pt.:
< 100 °C
Atm. press.:
>= 999 - <= 1 003 hPa
Decomposition:
no
Sublimation:
no

In the temperature range of 80 – 300 °C, an endothermic effect (boiling) was observed. No further thermal effects were observed up to the test end temperature of 500 °C.

 

Table 1:       Results of DSC Measurements

No.

Sample weight / mg

Onset of Effect / °C

Range of effect / °C

Weight loss / mg

PN13286

16.01

265.25

80 – 300 (endo)

16.10

PN13292

13.88

262.19

80 – 300 (endo)

13.91

 

During the cooling and the subsequent heating phase, no thermal effects were observed in the temperature range from -100 to 25 °C. It can be assumed that the test item has no melting or freezing point in this temperature range. Therefore the test item has no melting point down to a temperature of -100 °C.

 

Note: The difference between the recorded sample weight and recorded weight loss can be attributed to human error when recording the weight loss. This error does not affect the validity of the study as it is not a deviation from the prescribed technical guidance.

Conclusions:
The melting point/ freezing point of the test item is < -100 ℃.
Executive summary:

EU Method A.1. – The melting point/freezing point of the test item was determined using differential scanning calorimetry. 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 (0.0013 - 0.0016 g) were placed in crucibles and subjected to a thermal program from -100 °C to 500 °C. Cooling at a constant rate of 0.25 K/min was followed by a waiting period of 30 minutes at -100 °C and heating at a constant rate of 10 K/min to 500 °C. Two determinations were carried out. Both determinations were conducted under an inert atmosphere.  

 

The freezing temperature of the test item was established as being < - 100 °C.

Description of key information

Melting Point: < -100 °C; EU Method A.1.; H Smeykal (2017)

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:
-100 °C

Additional information

EU Method A.1. – The melting point/freezing point of the test item was determined using differential scanning calorimetry. 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 (0.0013 - 0.0016 g) were placed in crucibles and subjected to a thermal program from -100 °C to 500 °C. Cooling at a constant rate of 0.25 K/min was followed by a waiting period of 30 minutes at -100 °C and heating at a constant rate of 10 K/min to 500 °C. Two determinations were carried out. Both determinations were conducted under an inert atmosphere.  

 

The freezing temperature of the test item was established as being < - 100 °C.