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Melting point / freezing point

Link to relevant study record(s)

Reference

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

2019-2020

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Qualifier:

according to guideline

Guideline:

OECD Guideline 102 (Melting point / Melting Range)

Version / remarks:

1995

Deviations:

no

Qualifier:

according to guideline

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. QA statement)

Remarks:

Inspected on 15-16/11/2017, Signed on 15/05/2018

Type of method:

capillary method

Key result

Melting / freezing pt.:

>= -11 - <= 1.6 °C

Decomposition:

no

Sublimation:

no

Remarks on result:

other: pressure not specified

DSC Method

Pre-Test DSC

No event could be detected, the monitor was informed and the determinationof the freezing/melting point was conducted with the other methods.

Freezing Point Manual Method

Pre-Test Freezing Point

Values Pre-test Freezing Point

Subject	Temperature Test Item	Temperature Cooling Bath
Start of determination	22.6 °C	19.9 °C
Freezing Point	-35.5 °C	-40.8 °C

 

Observations test item:

-       Since 5 °C test item became very viscous, the resistance became stronger on the wire sling

-       Since 0 °C hardly possible to stir the wire sling, thereforethe temperature was observed without stirring, additionallythe surface of the test item was proved with a glass rod

-       Since -20 °C test item started to get solid

-       Since -35.5 °C solid like ice

Determination of the Freezing Point

Values Main Test Freezing Point – performed on 01. Apr. 2020

SubjectFirst determination	Temperature Test Item	Temperature Cooling Bath
Start of determination	21.3 °C	-40.7 °C
Freezing Point	-35.3 °C	-40.6 °C
Subject Second determination	Temperature Test Item	Temperature Cooling Bath
Start of determination	21.4 °C	-40.8 °C
Freezing Point	-35.4 °C	-40.9 °C

 

The observations were made like in the pre-test for freezing point.

Melting Point Capillary Method

The following values were recorded:

Values performed on 03. – 04. Apr. 2020

Melting range	Begin	End
First Determination	-10.9 °C (262.3 K)	1.7 °C (274.9 K)
Second Determination	-11.1°C (262.1 K)	1.5 °C (274.7 K)

 

Evaluationand Result

Freezing Point

The value of the mean was calculated as:

-35.4 ± 0.1 °C (237.8 ± 0.1 K)

Melting Point

The means between both determinations give the following values for the melting range:

Melting range:                         -11.0 to 1.6 °C (262.2 to 274.8 K)

Standard deviation:                  0.14 (begin); 0.14 (end)

Estimated accuracy:                ± 0.2 °C

 

2       Validity

2.1      Freezing Point

As the difference between the two values was found with 0.1 °C the validity criteria were met.

2.2      Melting Point

All validity criteria are presented in the following table.

Table 10.2‑a    Validity melting point

Parameter	Criterion	Found	Assessment
Difference between duplicate determinations	£0.5 K	0.2 K	valid
Difference between begin and end of melting process	£0.5 K	12.6 K	melting range was stated

 

Conclusions:

A freezing point was determined with–35.4 °C (237.8 K). A melting range was determined as-11.0 °C – 1.6 °C (262.2 to 274.8 K).

Executive summary:

An experimental study, conducted in accordance with conditions recommended in OECD guideline and under GLP was performed. The DSC- pre-test for determination of the freezing/melting point yield no reliable results.

Therefore, the determinations were performed with the other methods.

 The determination of the freezing point of the test item was determined with the Manual method. A freezing point was determined with–35.4 °C (237.8 K).

These values are the means of two independent determinations. The determination of the melting point of the test item was determined with the Capillary method.

A melting range was determined as-11.0 °C – 1.6 °C (262.2 to 274.8 K).

These values are the means of two independent determinations

 

As the test item is a liquid viscous UVCB substance it is not unusual that the DSC measurement could not find a reliable result. Often more energy is necessary as the DSC instrument can deliver to release the process of phase transition.

 

Anyway, no observations were made which might cause doubts on the validity of the study outcome. Therefore, the result of the study is considered valid.

Description of key information

A freezing point was determined with –35.4 °C (237.8 K). A melting range was determined as-11.0 °C – 1.6 °C (262.2 to 274.8 K).

Additional information

An experimental study, conducted in accordance with conditions recommended in OECD guideline and under GLP, was performed. It should be considered as a key study. The result should be retained as key data.