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Physical & Chemical properties

Melting point / freezing point

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Endpoint:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
supporting study
Study period:
04 - 12 Feb 2010
Reliability:
2 (reliable with restrictions)
Rationale for reliability incl. deficiencies:
guideline study with acceptable restrictions
Qualifier:
according to
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Version / remarks:
27th July 1995
Deviations:
yes
Remarks:
Only one temperature: -25 °C
Qualifier:
according to
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
Version / remarks:
18 march 2002
Deviations:
yes
Remarks:
Heating was omitted
Principles of method if other than guideline:
Deviations from guideline:
The sample is a fluid at +20 °C, so heating can be omitted
From literature it can be assumed, that the freezing point is under -20 °C.
For REACH the freezing point only has to be determined till a lower limit of -20 °C,so: A pour point analysis is performed at only one temperature: -25 °C
The measure to avoid super cooling was adding a few anti bumping granules.
The deviations will not lead to a different conclusion, only simplify the method
GLP compliance:
no
Type of method:
pour point
Melting / freezing pt.:
< 20 °C
Atm. press.:
101 325 Pa

After one week at -25 °C the surface of the substance moves, the substance is still fluid. A small rise in temperature may have occurred by removing the tubes from the freezer, but it is save to conclude the freezing point is below -20 °C for this substance.

Conclusions:
The pour point of the test substance is below -20 °C.
Endpoint:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
key study
Study period:
06 - 12 Apr 2010
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)
Version / remarks:
18 march 2002
Deviations:
no
Qualifier:
according to
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Version / remarks:
27th July 1995
Deviations:
no
GLP compliance:
no
Type of method:
differential scanning calorimetry
Remarks:
DSC
Melting / freezing pt.:
< -70 °C
Atm. press.:
101 325 Pa

Data below -70 °C are unreliable, as there is an effect of switching between the isothermal and heating stages. Similar effects as the ‘peak’ at -72 °C are observed, no matter what material or starting temperature. No melting, crystallization or glass transition can be assigned.

Conclusions:
The freezing point of the test substance is below -70 °C.

Description of key information

The freezing point of the substance is below -70 °C.

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:
-71 °C

Additional information

Hantink-de Rooij E.E.,2010, Determination of freezing point of Triethylenetetramine (TETA), Research, Development & Innovation AkzoNobel Arnhem, The Netherlands.

The pour point is below -20 °C

Hantink-de Rooij E.E.,2010,Determination of freezing point of Triethylenetetramine (TETA) with DSC, Research, Development & Innovation AkzoNobel Arnhem, The Netherlands.

Below -70 °C No melting, crystallization or glass transition can be assigned with scan rate 1 °C/min.

Both fair reports, according to OECD and EU guidelines, certificate of analysis in the reports.