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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:
03 - 15 January 2018
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Justification for type of information:
The study was conducted according to an internationally recognised method, and under GLP. The substance is considered to be adequately characterised. Therefore full validation applies.
Qualifier:
according to
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Version / remarks:
1995
Deviations:
no
Qualifier:
according to
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
Version / remarks:
2008
Deviations:
no
Principles of method if other than guideline:
Not applicable
GLP compliance:
yes (incl. certificate)
Remarks:
inspected on 15 and 16 November 2017 / signed on 15 May 2018
Type of method:
differential scanning calorimetry
Melting / freezing pt.:
< 5 °C
Atm. press.:
ca. 1 013 hPa

Results of the pre-test :

At room temperature, the test item was a slightly brown flowable liquid. At 5.0°, the test item was more solid compare to room temperature, but still pierceable (viscous mass). At -20.9°C and -80°C, the test item was solid.

Results of the Main test using DSC method:

In all runs the mass of the crucibles was the same and the crucible was visually unchanged.

In the cooling down phase no event could be detected, therefore the DSC measurements did not show any detectable freezing.

In the heating up phase two flat and wide events were detected. These events are endothermic. The detected events cannot clearly be identified.

The first event was observed in a range of -52.00 to -19.88 °C and the second in a range of -19.98 to 17.08 °C (evaluated with the event marker function).

These events might indicate a delay of melting. As the test item is a UVCB substance it is not unusual to have flat and wide peaks and even more as one peak. But it can be some kinds of transition as well.

As no freezing was observed during the cooling down phase, the events in the heating up phase cannot be considered as melting without ambiguity.

Therefore, the melting point of the test item has been stated based on the preliminary results, as below 5.0°C (278.2 K) under these circumstances.

No observations were made which might cause doubts on the validity of the study outcome.

Conclusions:
The melting point of test substance was determined to be below 5.0°C.
Executive summary:

The melting range of the test substance was determined under GLP according to EU Method A.1 and OECD 102, using the DSC method.

A pre-test was conducted, showing that the substance was a slightly brown flowable liquid at room temperature and atmospheric pressure. At 5.0°, the test item was more solid compare to room temperature, but still pierceable (viscous mass). At -20.9°C and -80°C, the test item was solid.

Third determinations were conducted by DSC including a replicate. In the cooling down phase no event could be detected, therefore the DSC measurements did not show any detectable freezing. In the heating up phase two flat and wide endothermic events were detected. The first event was observed in a range of -52.00 to -19.88 °C and the second in a range of -19.98 to 17.08 °C (evaluated with the event marker function). However, considering the complex nature of the test item and as no signs of freezing were observed during the cooling down phase, these events cannot clearly be identified. These events might indicate a delay of melting or some kinds of transition.

Finally, considering that in the pre-test, the test item was not frozen after a storage time of 24 hours at 5.0°C whereas it was frozen at -20.9 °C, the melting point of the test item was stated as below 5.0°C (278.2 K) under these circumstances.

Description of key information

The melting range of the test item was considered to be < 5.0°C (278.2K)

Key value for chemical safety assessment

Additional information

A fully reliable GLP experimental study, conducted according to a recognized OECD/EC guidelines is available.

It is considered as a key study.