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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:
2016-10-20 to 2016-11-23
Reliability:
2 (reliable with restrictions)
Rationale for reliability incl. deficiencies:
other: Performed according to relevant guidelines, however not compliant with GLP
Qualifier:
according to guideline
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Version / remarks:
adopted 1995-07-27
Deviations:
no
Qualifier:
equivalent or similar to guideline
Guideline:
other: ASTM D97
Version / remarks:
as referred to within OECD 102 for this specific method (pour point)
GLP compliance:
no
Other quality assurance:
other: The laboratory complied with a quality management system according to DIN EN ISO 9001 : 2008 and DIN EN ISO 14001 : 2009.
Type of method:
pour point
Specific details on test material used for the study:
LOT-Nr. 50000067900
Key result
Melting / freezing pt.:
-53 °C
Atm. press.:
1 013 hPa
Decomposition:
no
Sublimation:
no

Two measurements were performed:

Measurement 1:

Starting temperature: 0 °C

Result pour point: -53.0 °C

Measurement 1:

Starting temperature: -40 °C

Result pour point: -53.0 °C

Conclusions:
Pour point (OECD 102; ASTM D97): -53 °C (1013 hPa)
Executive summary:

The freezing point (pour point, determined according to OECD 102 and similar / equivalent to ASTM D 97) was determined to be -53.0 °C. Two measurements were performed, one starting at the initial temperature of 0°C, the other starting at -40 °C as the initial temperature. Both measurements had identical results (pour point -53.0 °C).

Description of key information

 Pour point (ASTM D97): -53 °C 

Key value for chemical safety assessment

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

Additional information

The pour point method was developed for use with petroleum oils and is suitable for use with oily substances with low melting temperatures. Because this applies to the test item, determination of the pour point is the most relevant method here. As the sample is cooled at a specific rate and examined at intervals of 3 K for flow characteristics and the lowest temperature at which movement of the substance is still observed is recorded as the pour point, it is actually a kind of freezing point. The pour point was determined according to ASTM D 97 with -53 °C from duplicate measurements yielding identical results (OXEA, 2016).

In addition, the melting point for the submission substance was determined by differential scanning calorimetry (DSC; Siemens, 2016). According to this method, the test item is first cooled down well below the freezing temperature and than heated up with a heating rate of 10 K/min up to 50 °C. An endothermal effect indicates melting. As such, indentification of the melting temperature approaches phase transition from the solid state temperature side by slowly increaing temperature, whereas pour point determination starts from liquid state temperature range to observe phase transition by stepwise decreasing temperature. As such, depending on the substance type, results for pour point and melting point may differ. This is indeed the case for the submission substance: the melting point determined by DSC was 8.0 °C, based on two experiments (7.91 °C measurement 1; 8.04 °C measurement 2).

This melting point is supported by a second study (Merieux, 2016), yielding a melting point of 9.1 °C (DSC, n=1).

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