Phenol, 4,4′-(1-methylethylidene)bis-, polymer with 2-(chloromethyl)oxirane and N1,N1-diethyl-1,3-propanediamine

Melting point / freezing point

Administrative data

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

05 February 2018 - 09 March 2018

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2018

Materials and methods

Test guideline

Test guideline 1

Qualifier:

according to guideline

Guideline:

EU Method A.1 (Melting / Freezing Temperature)

Version / remarks:

2016

Deviations:

no

Test guideline 2

Qualifier:

according to guideline

Guideline:

OECD Guideline 102 (Melting point / Melting Range)

Version / remarks:

1995

Deviations:

no

Test guideline 3

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

Test material

Test material information

Constituent 1

Reference substance name:

DEPDA adduct

Cas Number:

123739-10-6

IUPAC Name:

DEPDA adduct

Test material form:

solid

Details on test material:

- Physical appearance: dark amber solid
- Storage conditions: at room temperature

Results and discussion

Melting / freezing point

Key result

Decomposition:

yes

Decomp. temp.:

300 °C

Remarks on result:

other: Glass transition point: 18.3°C. No melting/freezing point was determined between -50°C and decomposition.

Any other information on results incl. tables

TGA EXPERIMENT (PRELIMINARY TEST)

Significant decrease of weight from 325°C upwards. 25% weight loss at 364°C and 70% weight loss at 477°C.

After the experiment, a dark brown molten residue remained in the sample container (original colour: dark amber). The change of the colour indicated reaction and/or decomposition of the test item.

DSC EXPERIMENT 1

A glass transition was observed directly followed by an endothermic effect between 0°C and 175°C. The inflection point of the glass transition was 17.527°C. Based on the small weight loss observed during the preliminary test, the endothermic effect was due to evaporation of volatile components from the test item which is a mixture of compounds. An exothermic peak was observed starting at 300°C. The exothermic effect was due to reaction and/or decomposition of the test item. After the experiment, an orange/brown molten residue remained in the sample container.

DSC EXPERIMENT 2

To investigate the effectsbetween 0°C and 175°C,a repeated heating cycle was applied in the Experiment 2. With the first heating theinflection point of the glass transition was 19.409°C. During cooling, a glass transition between 0°C and 50°C was found. With the second heating, the inflection point was 19.201°C. This inflection point was not used for calculating the melting temperature, since it was obtained during the second heating of the experiment. The endothermic effect was not observed during the second heating, indicating that evaporation of volatile components was the reason for the effect. After the experiment, a dark yellow molten residue remained in the sample container.

DSC EXPERIMENT 3

The inflection point of the glass transition was now 18.069°C. After the experiment, a dark yellow molten residue remained in the sample container. 

DATA HANDLING

The glass transition temperature was determined as the mean inflection point of Experiment 1, Experiment 2 and Experiment 3

 

DSC and TGA graphs: see Attachement

Applicant's summary and conclusion

Conclusions:

A glass transition temperature of 18.3°C was determined. The substance has no melting/freezing temperature between -50°C and decomposition at 300°C

Executive summary:

Differential Scanning Calorimetry (DSC) experiments were performed in a GLP study according to EC A.1, OECD 102 and OPPTS 830.7200.

The substance has no melting/freezing temperature between -50°C and decomposition. From triplicate measurements the mean glass transition temperature was determined to be 18.3°C.

Reaction and/or decomposition of the substance started at 300°C.