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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:
27 March 2017 - 09 January 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:
July 1995
Deviations:
no
GLP compliance:
yes (incl. QA statement)
Type of method:
differential scanning calorimetry
Key result
Melting / freezing pt.:
< -100 °C
Atm. press.:
>= 999 - <= 1 002.8 hPa
Decomposition:
no
Sublimation:
no
Remarks on result:
other: Mean value.
Remarks:
Arising from 3 determinations.

No.

Sample weight / mg

Onset of Effect / °C

Range of effect / °C

Weight loss / mg

Atmospheric pressure / hPa

PN13287

13.03

-26.37

-30 – 0 (endo)

9.77

999.0

96.70

30 – 160 (endo)

182.38

180 – 260 (endo)

274.66

260 – 280 (endo)

---

280 – 410 (exo)

PN13300

17.72

-22.33

-30 – 0 (endo)

13.20

1002.8

107.74

70 – 150 (endo)

241.92

200 – 260 (endo)

274.01

260 – 280 (endo)

---

280 – 320 (exo)

PN13476

18.37

-30.93

-40 – 0 (endo)

14.68

1001.3

105.43

70 – 150 (endo)

244.37

150 – 250 (endo)

258.94

250 – 280 (endo)

---

280 – 320 (exo)

 

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

During the heating phase a very small endothermic effect was observed in the temperature range of -40 to 0 °C.

These endothermic effects were investigated. 6.6 g of the test item was cooled in a test tube using liquid nitrogen to approx. -60 °C. At approx. -30 °C the test item changed consistency and colour, from a very viscous transparent liquid to a white mass (without achieving a solid state). When warmed from -60 °C to ambient temperature, the appearance of the test item returned to being a viscous and transparent liquid at approx. -20 °C. From these observations, it can be concluded these endothermic effects are not associated with melting or freezing as a phase transition did not occur.

 

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 - 0.0018 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. Three determinations were carried out. All 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 - 0.0018 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.  Three determinations were carried out.  All determinations were conducted under an inert atmosphere.  

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