Reaction mass of 2-ethylhexyl (3-isocyanato-4-methylphenyl)carbamate and 2-ethylhexyl (5-isocyanato-2-methylphenyl)carbamate and 2-ethylhexyl (3-isocyanato-2-methylphenyl)carbamate

Boiling point

Link to relevant study record(s)

Reference

Endpoint:

boiling point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

22. May 2018 to 29. May 2018

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Qualifier:

according to guideline

Guideline:

OECD Guideline 103 (Boiling Point)

Version / remarks:

OECD Guideline No. 103 “Boiling Point“, dated 27. Jul. 1995

Deviations:

no

Qualifier:

according to guideline

Guideline:

EU Method A.2 (Boiling Temperature)

Version / remarks:

EU-Method A.2 dated 31. May 2008, “Boiling Temperature“

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Type of method:

differential scanning calorimetry

Specific details on test material used for the study:

No further details specified in the study report.

Key result

Boiling pt.:

> 317.74 - < 328.68 °C

Decomposition:

yes

Decomp. temp.:

331.36 °C

Remarks on result:

other: Atm. press. not specified

Pre-test following Siwoloboff

All observations of the Pre-test following Siwoloboff are presented in the following table.

Pre-test following Siwoloboff

Temperature °C	Observations
73	Singular bubbles, which were into the test item, rose
115	Residual bubbles, which were into the test item, rose
171	Singular bubbles rose
260	Colour got darker (more yellow)
281	Divers singular bubbles rose
292	Divers bubbles and colour got darker (orange)
297	Many bubbles rose and the colour got darker (brown)
313	Chain of bubbles were observed, gas burner switched off
296	Broke of the chain of bubbles were observed

 

After cooling down the test item changed the colour into dark-brown

 

Security Pre-test for the DSC instrument

The crucible was found visually unchanged after reaching a temperature of 450 °C. The weight of the crucible was recorded with 46.40 mg.

 

Calibration

Values DSC Indium

Expected Melting point	Measured Melting point	Expected Energy	Measured Energy	Assessment
156.6 ± 1.0 °C	156.44 °C (onset)	28.45 ± 1.0 J/g	29.39 J/g	OK

The measurement of indium after calibration met the validity criteria.

 

DSC Measurement of the Test item

First determination

As not the whole event could be detected the temperature range was adapted from 25 to 400 °C.

After the measurement the crucible was opened and a yellow-green residue was left.

 

Second determination

The crucible was gold brown coloured with test item around the perforation after the measurement. The crucible was opened and a red residue was left.

 

Values DSC Test item second determination

[°C]	Temperature [°C]	Energy
Boiling Point Begin End Peak max.	328.68 (onset) 269.78 (Event marker) 370.02 (Event marker) 329.21 (Event marker)	332.95 [J/g] 17.68 mW 13.05 mW 40.28 mW

 

Third determination

The crucible was gold brown coloured with test item around the perforation after the measurement. The crucible was opened and a red residue was left.

 

Values DSC Test item third determination

[°C]	Temperature [°C]	Energy
Boiling Point Begin End Peak max.	317.74 (onset) 284.72 (Event marker) 363.18 (Event marker) 331.36 (Event marker)	339.53 [J/g] 17.37 mW 12.94 mW 17.57 mW

 

To ensure the measured values a further measurement was performed.

 

Fourth determination

Values DSC Test item fourth determination

[°C]	Temperature [°C]	Energy
Boiling Point Begin End Peak max.	318.70 (onset) 287.64 (Event marker) 364.34 (Event marker) 329.82 (Event marker)	340.26 [J/g] 19.35 mW 15.58 mW 16.95 mW

 

Observations

Values Observations

	Mass test item	Mass crucible (before measurement):	Mass crucible (after measurement):	Observations
First Measurement	10.33 mg	56.06 mg	53.91 mg	After the test the crucible was visually unchanged
Second Measurement	8.95 mg	54.77 mg	47.03 mg	After the test the crucible was gold brown coloured with test item around the perforation
Third Measurement	6.10 mg	51.13 mg	45.82 mg	After the test the crucible was visually unchanged
Fourth Measurement	5.75 mg	51.22 mg	46.29 mg	After the test the crucible was visually unchanged

 

Interpretation of the measurements

Four DSC measurements were performed. The first is not evaluated as not the whole event could be detected. In the measurements 2 – 4 one endothermic event was detected which can be identified as boiling point according to the observations of the pre-test.

In the second DSC run probably superheating have occurred which cause the sharp peak in the DSC curve and the observed contamination of the crucible after the measurement.

In the third and fourth measurement less test item was used which caused similar curves.

Clearly signs of decomposition were observed, like in the pre-test as well (Colour change in the pre-test, residue in the crucibles).

Therefore, boiling under decomposition should be stated in a range (Onset).

Conclusions:

The determination of the boiling point Trixene AS was performed via DSC (differential scanning calorimetry). In all runs one event was detected.
The event is endotherm and is stated as the boiling under decomposition.
The results of the study should be stated as followed:
317.74 to 328.68 °C (590.89 to 601.83 K)
Decomposition was indicated by colour change of the test item.
A peak maximum was detected with 331.36 °C (604.51 K).
The whole event was measured in a range of 269.78 to 370.02 °C (542.93 to 643.17 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.

Executive summary:

Determination of the boiling point of Trixene AS according to OECD 103 resp. EU A.2

 

Findings and Results:

The determination of the boiling point Trixene AS was performed via DSC (differential scanning calorimetry). In all runs one event was detected.

The event is endotherm and is stated as the boiling under decomposition.

The results of the study should be stated as followed:

317.74 to 328.68 °C (590.89 to 601.83 K)

Decomposition was indicated by colour change of the test item.

A peak maximum was detected with 331.36 °C (604.51 K).

The whole event was measured in range of 269.78 to 370.02 °C (542.93 to 643.17 K)

Description of key information

The results of the study should be stated as followed:

317.74 to 328.68 °C (590.89 to 601.83 K)

Key value for chemical safety assessment

Boiling point at 101 325 Pa:

328.68 °C

Additional information

The determination of the boiling point Trixene AS was performed via DSC (differential scanning calorimetry). In all runs one event was detected. The event is endotherm and is stated as the boiling under decomposition.

The results of the study should be stated as followed:

317.74 to 328.68 °C (590.89 to 601.83 K)

Decomposition was indicated by colour change of the test item.

A peak maximum was detected with 331.36 °C (604.51 K).

The whole event was measured in range of 269.78 to 370.02 °C (542.93 to 643.17 K)