7-azatridecane-1,13-diamine

Boiling point

Link to relevant study record(s)

Reference

Endpoint:

boiling point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

2018-02-01 to 2018-03-06

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Qualifier:

according to guideline

Guideline:

OECD Guideline 103 (Boiling Point)

Version / remarks:

Adopted: 1995-07-27

Deviations:

no

Qualifier:

according to guideline

Guideline:

EU Method A.2 (Boiling Temperature)

Version / remarks:

March 04, 2016

Deviations:

no

Qualifier:

according to guideline

Guideline:

EPA OPPTS 830.7220 (Boiling Point / Boiling Range)

Version / remarks:

August 1996

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Type of method:

differential scanning calorimetry

Key result

Boiling pt.:

330.9 °C

Atm. press.:

1 024 hPa

Decomposition:

no

Results

A) Preliminary Test

The TGA curve of the test item was determined. Starting at 200°C, the weight of the sample decreased significantly. At 255°C, the sample weight had decreased by 25%.

After the experiment it was observed that the test item had evaporated from the sample container.

B) Main Study

From the DSC curve obtained with Experiment 1 an endothermic peak was observed between 0°C and 50°C directly followed by a broad endothermic effect between 50°C and 150°C.  The extrapolated onset temperature of the first peak was 31.007°C.  The first endothermic effect was most likely obtained due to melting of the test item.  Based on the weight loss observed during the preliminary test, the second endothermic effect was due to evaporation of volatile components.  A third endothermic peak was observed between 250°C and 350°C.  The extrapolated onset temperature of this boiling peak was estimated to be 302.917°C.  The amount of material used was not sufficient for accurate determination of the boiling temperature.  After the experiment it was observed that the test item had evaporated from the sample container.

In order to investigate the melting peak, Experiment 2 was stopped directly after the melting peak. From the obtained DSC curve the extrapolated onset temperature was 30.409°C.  After the experiment, a white molten residue remained in the sample container (original colour: off white).  It demonstrated that melting was the reason for the endothermic effect.

In order to investigate the boiling peak, a higher heating rate of 50°C/minute was used in the Experiment 3.  From the obtained DSC curve the extrapolated onset temperature of the melting peak was 35.191°C.  The extrapolated onset temperature of the boiling peak was 329.783°C.  After the experiment it was observed that the test item had evaporated from the sample container.   Experiment 4 and Experiment 5 showed that in Experiment 3 the boiling peak had not shifted to higher temperatures due to the higher heating rate.  It demonstrated that boiling of the test item caused the endothermic effect.  Since however a higher heating rate was applied in Experiment 3, the extrapolated onsets of Experiment 3 were not used for calculation of the melting and boiling temperature of the test item.    

In order to determine the boiling temperature, a higher amount of test item was used in the Experiment 4.  From the corresponding DSC curve (see attached illustration) the extrapolated onset temperature of the melting peak was 30.421°C.  The extrapolated onset temperature of the boiling peak was 330.480°C.  After the experiment it was observed that the test item had evaporated from the sample container.

Experiment 5 was performed as a duplicate of Experiment 4.  From the obtained DSC curve the extrapolated onset of the melting peak was 31.394°C.  The extrapolated onset of the boiling peak was 331.229°C.  After the experiment it was observed that the test item had evaporated from the sample container.

The melting temperature was determined as the mean melting temperature of Experiment 1 (31.007°C), Experiment 2 (30.409°C), Experiment 4 (30.421°C) and Experiment 5 (31.394°C).  The difference between the observed melting temperatures was most likely due to the evaporation of volatile components which might affected the shape of the melting peaks.

The boiling temperature was determined as the mean boiling temperature of Experiment 4 (330.480°C) and Experiment 5 (331.229°C).

Conclusions:

The boiling temperature of Bis(hexamethylene)triamine was determined by DSC.
The boiling temperature of the test item was 330.9°C (604.0 K) (arithmetic mean value; n= 2).

Executive summary:

The boiling point of the test item Bis(hexamethylene)triamine was determined by DSC according to OECD 103 and EU method A.2, compliant with GLP.

The boiling point was determined from two valid DSC experiments (heating rate: 20 °C per minute) as the arithmetic mean value of extrapolated onset temperatures: 330.9 °C (604.0 K).

This value is based on the following results: Experiment 4 (330.480 °C), Experiment 5 (331.229 °C).

Description of key information

The boiling temperature of Bis(hexamethylene)triamine was determined by DSC.

The boiling temperature of the test item was 330.9 °C (604.0 K) (arithmetic mean value; n= 2).

Key value for chemical safety assessment

Boiling point at 101 325 Pa:

330.9 °C

Additional information

The boiling point of the test item Bis(hexamethylene)triamine was determined by DSC according to OECD 103 and EU method A.2, compliant with GLP.

The boiling point was determined from two valid DSC experiments (heating rate: 20 °C per minute) as the arithmetic mean value of extrapolated onset temperatures: 330.9 °C (604.0 K).

This value is based on the following results: Experiment 4 (330.480 °C), Experiment 5 (331.229 °C).