4,4'-methylenebis[N-sec-butylaniline]

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:

from 10 April 2018 to 20 June 2018

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Reason / purpose for cross-reference:

reference to same study

Qualifier:

according to guideline

Guideline:

EU Method A.1 (Melting / Freezing Temperature)

Version / remarks:

2016

Deviations:

no

Qualifier:

according to guideline

Guideline:

OECD Guideline 102 (Melting point / Melting Range)

Version / remarks:

1995

Deviations:

no

Qualifier:

according to guideline

Guideline:

EPA OPPTS 830.7200 (Melting Point / Melting Range)

Version / remarks:

1998

Deviations:

no

GLP compliance:

yes

Type of method:

differential scanning calorimetry

Key result

Atm. press.:

>= 1 014 - <= 1 024 hPa

Remarks on result:

other: Glass transition point: -45.6°C. The substance has no melting/freezing temperature between 25°C and -90°C.

DSC EXPERIMENT 1

During cooling, a glass transition was observed between -80°C and -40°C. During heating, a glass transition was observed between -50°C and -25°C. The inflection point of the glass transition was -45.675°C. An endothermic peak was observed starting at 300°C. After the experiment, a colourless residue remained in the sample container.

DSC EXPERIMENT 2

In order to investigate the endothermic peak observed from 300°C, Experiment 2 was stopped at 500°C. The inflection point of the glass transition was -45.425°C. The extrapolated onset temperature of the endothermic peak was 424.540°C. After the experiment it was observed that the test item had evaporated from the sample container. DSC curve during heating: see illustration below.

DSC EXPERIMENT 3

In order to further investigate the endothermicpeak, a higher heating rate of 50°C/minute was used in Experiment 3. The extrapolated onset temperature was 426.160°C. The endothermic peak had not shifted to significantly higher temperatures. It demonstrated that boiling of the test item caused the endothermic effect. After the experiment it was observed that the test item had evaporated from the sample container.

DSC EXPERIMENT 4

Experiment 4 was performed to determine the duplicate boiling temperature. The extrapolated onset of the boiling peak was 424.981°C. After the experiment it was observed that the test item had evaporated from the sample container.

DATA HANDLING

-The glass transition temperature was determined as the mean inflection point of Experiment 1 and Experiment 2.

-The boiling temperature was evaluated from the DSC curve as the extrapolated onset temperature of the endothermic boiling peak: mean of Experiment 2 (424.540°C) and Experiment 4 (424.981°C).

 

Conclusions:

A glass transition temperature of -45.6°C was determined. The substance has no melting/freezing temperature between 25°C and -90°C. The boiling temperature was determined to be 424.8°C (at 1019 ± 5 hPa).

Executive summary:

Differential Scanning Calorimetry was performed to determine the melting and boiling temperature. The experiments were based on EC A.1, OECD 102 and OPPTS 830.7200 (melting temperature) and on EC A.2, OECD TG 103 and OPPTS 830.722 (boiling temperature). GLP-study.

The liquid substance has no melting/freezing temperature between 25°C and -90°C. DSC showed glass transition. From duplicate measurements a mean glass transition temperature was determined to be -45.6°C.

From two DSC experiments, the mean boiling temperature was determined to be 424.8°C (at 1019 ± 5 hPa).

Description of key information

Glass transition temperature: -45.6°C (EC A.1, OECD 102, OPPTS 830.7200: DSC)

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:

-45.6 °C

Additional information

no melting/freezing temperature between 25°C and -90°C