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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 08 march 2018 to 20 september 2018
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Qualifier:
according to guideline
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
Qualifier:
according to guideline
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Qualifier:
according to guideline
Guideline:
other: ISO 11357-1. (2016). Plastics
Version / remarks:
Differential Scanning Calorimetry (DSC) – Part 1: General principles. CEN, Bruxelles.
Qualifier:
according to guideline
Guideline:
other: ISO 11357-3. (2013). Plastics
Version / remarks:
Differential Scanning Calorimetry (DSC) – Part 3: Determination of temperature and enthalpy of melting and crystallization. CEN, Bruxelles.
GLP compliance:
yes (incl. QA statement)
Type of method:
differential scanning calorimetry
Specific details on test material used for the study:
SOURCE OF TEST MATERIAL
- Source and lot/batch No.of test material: 80555E094
- Expiration date of the lot/batch: 05 December 2018
- Manufacturing test date: 05 December 2017
Melting / freezing pt.:
-85.4 °C
Atm. press.:
978 hPa
Melting / freezing pt.:
-85 °C
Atm. press.:
977 hPa
Key result
Melting / freezing pt.:
-85.2 °C
Atm. press.:
978 hPa

Temperature program:

Pre-Study : Peaks assigned to the boiling of the substance were observed and measurement was stopped at 435°C

First determination with Atmospheric pressure 978.0 hPa :

The melting point was observed at -85.4°C (onset temperature of the first peak)

The initial boiling point was observed at 269.1 °C (onset temperature of the second peak) and a corresponding mass loss is observed on the TG curve, showing that all the substance was evaporated at the end of the study.

The crucible was visually checked after the determination: By opening the crucible, no test item left in the crucible and no sign of decomposition was observed.

Second Determination with Atmospheric pressure 977.0 hPa :

The melting point was observed at -85.0°C (onset temperature of the first peak)

 The initial boiling point was observed at 269.4 °C (onset temperature of the second peak) and a corresponding mass loss is observed on the TG curve, showing that all the substance was evaporated at the end of the study.

The crucible was visually checked after the determination: By opening the crucible, no test item left in the crucible and no sign of decomposition was observed.

The apparatus is checked with the reference substance Indium.

For temperature, the expected melting point: 156.6 +/- 0.5°C(reference value rounded up due to the temperature resolution of the apparatus used)

Obtained melting point: 156.6°C

The melting point of the Indium respects the defined tolerance of the expected melting point.

For sensitivity, the expected enthalpy: 28.6 +/- 2.9 J/g

Obtained enthalpy: 28.11 J/g

The enthalpy of the indium respects the defined tolerance of the expected enthalpy.

Conclusions:
The melting point of test item was determined using a Differencial Scanning Calorimetry (DSC) and following the OECD Guideline 102, "Melting Point/Melting Range" and the Regulation EC No. 440/2008 Method A.1.
The melting point of the substance was determined to be -85.2 °C at ambient pressure (978.0 hPa).
Executive summary:

In this method, two crucibles were put in the apparatus furnace under inert atmosphere (helium) at atmospheric pressure. One crucible contained the test item, the other was empty and considered as the reference. A specific temperature program was applied.

The crucibles were linked to two thermocouples fixed on the TG-DSC sample carrier. Heat flow differences between the two crucibles and mass variation were recorded on a thermogram.

A cooling system usingliquid nitrogen allowed experiments with low temperatures down to -120°C.

Two trials were conducted and corresponding thermograms were obtained.

The melting point values respect validity criteria (less than 0.5 °C of difference up to 326.85°C) and the melting point of the Indium reference respects the checking cards limits so as its enthalpy.

Description of key information

The melting point of test item was determined using a Differencial Scanning Calorimetry (DSC) and following the OECD Guideline 102, "Melting Point/Melting Range" and the Regulation EC No. 440/2008 Method A.1.

The melting point of the substance was determined to be  -85.2 °C at ambient pressure (978 hPa).

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:
-85.2 °C

Additional information