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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:
From 16 December 2011 to 3 September 2012
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Remarks:
Study conducted in compliance with international and OECD standard guidelines under GLP conditions. The study report was well documented with all mandatory information included.
Qualifier:
according to guideline
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Deviations:
no
Qualifier:
according to guideline
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
Deviations:
no
GLP compliance:
yes (incl. QA statement)
Remarks:
2011-08-31
Type of method:
method to determine freezing temperature
Melting / freezing pt.:
< -20 °C
Remarks on result:
other: the test item became slightly viscous during cooling

Results of determination 1 :






















































































































































time of cooling (s)



temperature of cooling (°K)



time of cooling (s)



temperature of cooling (°K)



time of cooling (s)



temperature of cooling (°K)



0



295



510



276



1020



266



30



293



540



275



1050



266



60



292



570



275



1080



265



90



290



600



274



1110



265



120



289



630



274



1140



264



150



287



660



273



1170



264



180



286



690



272



1200



263



210



285



720



272



1230



263



240



2853



750



271



1260



262



270



282



780



271



1290



262



300



281



810



270



1320



261



330



281



840



269



1350



261



360



280



870



269



1380



260



390



279



900



268



1410



260



420



278



930



268



1440



259



450



277



960



267



1470



259



480



277



990



267



1500



259



 


















































































































time of cooling (s)



temperature of cooling (°K)



time of cooling (s)



temperature of cooling (°K)



1530



258



2040



254



1560



258



2070



253



1590



258



2100



253



1620



257



2130



253



1650



257



2160



253



1680



257



2190



253



1710



256



2220



253



1740



256



2250



253



1770



256



2280



252



1800



256



 



 



1830



255



 



 



1860



255



 



 



1890



255



 



 



1920



255



 



 



1950



254



 



 



1980



254



 



 



2010



254



 



 



 The test item became slightly viscous during cooling. Freezing temperature is less than 20°C (<253°K)


 


Results of determination 2:






















































































































































time of cooling (s)



temperature of cooling (°K)



time of cooling (s)



temperature of cooling (°K)



time of cooling (s)



temperature of cooling (°K)



0



294



510



270



1020



258



30



293



540



269



1050



257



60



291



570



268



1080



257



90



289



600



267



1110



256



120



287



630



266



1140



255



150



285



660



266



1170



255



180



284



690



265



1200



254



210



282



720



264



1230



254



240



281



750



263



1260



254



270



279



780



263



1290



254



300



278



810



262



1320



253



330



277



840



261



1350



253



360



276



870



261



1380



253



390



275



900



260



1410



253



420



273



930



260



1440



252



450



272



960



259



 



 



480



271



990



258



 



 



The test item became slightly viscous during cooling. Freezing temperature is less than - 20°C (<253°K).


Graphs of temperature (K) versus time (seconds) for determination 1 and 2 are shown in the attached illustration

Conclusions:
The freezing temperature of the test item has been determined to be less than -20°C (<253K).
Executive summary:

The determination of the freezing point was carried out according to the Method A1 Melting/Freezing Temperature of Commission Regulation (EC) N°440/2008 of 30 May 2008, Method 102 of the OECD Guidelines for Testing of Chemicals, 27 July 1995 and according to GLP. No deviation from the guideline was observed during the test.


An aliquot (approximately 15 mL) of test item was placed into a test tube containing a thermometer. A wire loop with which the sample could be agitated was placed inside the tube to ensure sample homogeneity during cooling. The test tube was surrounded by a glass jacket and then placed into a large beaker containing a dry ice/acetone mixture. The temperature and observations of the test item were recorded every 30 seconds. The dry ice/acetone bath was maintained until the sample temperature had reached at least -20°C or until the test item solidified.


The test item became slightly viscous during cooling but did not solidify during both determinations down to -20°C. In accordance with Column 2 of the Annex VII of REACH, Information requirement section 7.2, this study does not need to be conducted below a lower limit of -20°C. So the freezing temperature of the test item has been determined to be less than -20°C (<253K).

Description of key information

Experimental value of freezing point : < -20°C (<253K).

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:
-20 °C

Additional information

The determination of the freezing point was carried out according to the Method A1 Melting/Freezing Temperature of Commission Regulation (EC) N°440/2008 of 30 May 2008, Method 102 of the OECD Guidelines for Testing of Chemicals, 27 July 1995 and according to GLP.


The test item became slightly viscous during cooling but didn't solidify during determinations down to -20°C. In accordance with Column 2 of the Annex VII of REACH, Information requirement section 7.2, this study does not need to be conducted below a lower limit of -20°C.

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