4,4'-methylenebis(2,6-xylidine)

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:

05 - 13 February 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. Test substance is adequately characterised. Therefore full validation applies.

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 13 and 14 October 2014/ Signed on 8 April 2015

Type of method:

differential scanning calorimetry

Key result

Melting / freezing pt.:

>= 119.47 - <= 121.44 °C

Decomposition:

no

Pre-Test

The capillary tube containing the test item was set into the block at 18.6 °C. The block was heated until melting started. The temperature was noted at which the first signs of melting of the test item were observed. When the test item was completely melted, the temperature was noted again.

 

Table 4.2 /1.- Results of the pre-test

Observations	Temperature
The test item began to melt to a clear liquid.	119 °C
The test item was nearly melted, only on the surface some particles left	127 °C
Completely clear liquid	130 °C

 

After cooling down test item solidified to a white solid again.

Security Pre-test for the DSC instrument

Thecrucible was bloated after reaching a temperature of 420 °C. No further heating was performed.

The weight of the crucible was recorded with 36.11 mg.

Observations

Table 4.2/2.-Values Observations

	Mass test item	Mass crucible (before measurement):	Mass crucible (after measurement):	Observations
First Measurement	2.03 mg	59.74 mg	59.73 mg	The crucible was visual unchanged after measurement
Repetition Second Measurement	First crucible	59.73 mg	59.74 mg
Third Measurement	2.48 mg	47.65 mg	47.74 mg

 

The first and the second crucible were opened after measurement. In the first crucible a yellow-orange residue was left. In the second crucible the residue looked like in the original state.

Interpretation

In all DSC runs one endothermic peak was detected, which can be identified as a melting peak. The pre-test confirmed this.

Presentation of results

For the evaluation the values of the first and third determination were taken, as the second measurement showed difference in curve and results. The evaluation was made with the Onset function of the software.

Table 4.2/3.- Values Results

Melting Range	in °C	in K
First determination	121.44	394.59
Third determination	119.47	392.62
Min	119.47	392.62
Max	121.44	394.59

 

Validity

As the deviation between the two evaluated determinations (first and third determinations) is above 0.5 K a melting range is stated.

 

Discussion

The determination of the melting point of the test item was performed via DSC (differential scanning calorimetry). In all runs one event was detected. The event is endothermic and is stated as a melting range with 119.47 (392.62 K) to 121.44 (394.59 K).

These values are the results of two independent determinations.

 

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

 

Conclusions:

The melting range of the test item is stated as: 119.47°C (392.62 K) to 121.44°C (394.59 K).

Executive summary:

This study (was performed in order to determine the melting range of the test item according OECD 102 resp. EU A.1.

The melting point was determined via DSC (differential scanning calorimetry). The melting range was determined under these circumstances as the endothermic event with 119.47 (392.62 K) to 121.44 (394.59 K). These values are the results of two independent determinations.

Description of key information

The melting range of the test item is stated as: 119.47°C (392.62 K) to 121.44°C (394.59 K).

Additional information

A fully reliable experimental study, conducted according to OECD 102/ EU A1 guideline is available.

It is considered as a key study, and the result is retained as key data.