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

Boiling point

Link to relevant study record(s)

Reference

Endpoint:

boiling point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

5 - 28 Mars 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 103 (Boiling Point)

Version / remarks:

1995

Deviations:

no

Qualifier:

according to guideline

Guideline:

EU Method A.2 (Boiling 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

Boiling pt.:

417.33 °C

Atm. press.:

ca. 101.3 kPa

Decomposition:

yes

Remarks:

The observed lowering of the baseline and the changed appearance of the test item in the crucible after measurement may indicate a decomposition of the test item.

Remarks on result:

other: During the pre-test possibly signs of decomposition were observed indicated by colour change.

Results

Pre-test following Siwoloboff

The following observations were noted:

Table 4.3/1.- Observations Pre-test

Observations	Temperatures
Test item compacted slightly	74 °C
Test item become yellow on the bottom and begin to melt	123 °C
Completely melted to slightly yellow liquid	141 °C
Test item become more yellow	187 °C
Slowly colour change to dark yellow till slightly orange	224 °C
Colour dark orange till brown	266 °C
Colour chestnut brown	280 °C
Test stopped no signs for boiling; only getting darker.	400 °C

 

Security Pre-test for the DSC instrument

The crucible was found visual unchanged after reaching a temperature of 450°C. The weight was recorded with 54.33 mg. After further heating to 600°C and cooling down the crucible was strongly bloated and the edge of the crucible was black discolored. The weight was recorded with 45.71 mg.

Presentation of results

Table 4.3/2.- Values results

Boiling Point	in °C	in K
1DeterminationOnset	417.33	690.48
2DeterminationOnset	417.32	690.47
Mean	417.33	690.48
Standard deviation	0.01	0.01

Observations

Table 4.3/3.- Values Observations

	Mass test item	Mass crucible (before measurement):	Mass crucible (after measurement):	Observations
First Measurement	8.03 mg	53.76 mg	45.73 mg	After the test the crucible was visually unchanged
Second Measurement	8.71 mg	53.82 mg	45.30 mg

 

Both crucibles were opened after measurement a yellow residue was left.

Interpretation of the measurements

In both DSC runs two endothermic peaks were detected.

The first peak was already identified as the melting point (see if necessary endpoint 4.2).

Therefore the second peak can be identified as the boiling point.

The observed lowering of the baseline and the changed appearance of the test item in the crucible after measurement may indicate a decomposition of the test item.

Validity

As the difference between the two evaluated determinations for the boiling point was below 0.5 K the result can be considered valid.

Conclusions:

The boiling point of the test item with signs of decomposition is stated as: 417.33 ± 0.01 °C (690.48 ± 0.01 K)

Executive summary:

The study was performed in order to determine the boiling point of test item according to OECD 103, resp EU A.2 guideline.

The determination of the boiling point of the test item was performed via DSC (differential scanning calorimetry). In all runs two events were detected.

The events are endotherm.

The first one is the melting point and the second one is the boiling point. The boiling point under these circumstances with signs of decomposition should be stated as followed: 417.33 ± 0.01 °C (690.48 ± 0.01 K).

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

The boiling point under these circumstances with signs of decomposition should be stated as followed: 417.33 ± 0.01 °C (690.48 ± 0.01 K)

Key value for chemical safety assessment

Boiling point at 101 325 Pa:

417.33 °C

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.