Reaction productReaction product of 1,1´-Methylenebis(4-substituted cyclohexane), [2-(substitutedmethyl)-3-prop-2-enoyloxy-2-(prop-2-enoyloxymethyl)propyl] prop-2-enoate and [3-prop-2-substituted-2,2-bis(prop-2-enoyloxymethyl)propyl] prop-2-enoate

Melting point / freezing point

Administrative data

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

03 January 2012- 19 March 2012

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

other: The study has been performed according to OECD and EC guidelines and according to the principles of GLP.

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2012

Report date:

2012

Materials and methods

Test guideline

Test guideline 1

Qualifier:

according to guideline

Guideline:

EU Method A.1 (Melting / Freezing Temperature)

Version / remarks:

(2008)

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:

other: OECD Guideline 113 (Thermal stability) (1981)

GLP compliance:

yes (incl. QA statement)

Type of method:

thermal analysis

Remarks:

differential scanning calorimetry

Test material

Test material information

Constituent 1

Details on test material:

- Physical state: Clear colourless/slightly yellow, sticky resin
- Stability under test conditions: Stable
- Storage condition of test material: At room temperature protected from light
- Stability at higher temperatures: Maximum 1 month at 50°C
- General information: Avoid heat, direct sunlight, acid and base

Results and discussion

Melting / freezing point

Melting / freezing point 1

Melting / freezing pt.:

-19 °C

Remarks on result:

other: glass transition

Melting / freezing point 2

Melting / freezing pt.:

254 K

Any other information on results incl. tables

Preliminary TGA:

The TGA-curve of the test substance is shown in Figure 1 of the study report (see attachment). At 150°C, the weight of the sample started to decrease. From 400°C upwards the weight of the sample decreased significantly. At 435°C the sample weight had decreased by 25%. After the experiment, a black residue remained in the sample container (originally colourless or slightly yellow). The change of the colour indicated reaction and/or decomposition of the test substance.

DSC experiments:

Experiment 1: a glass transition was observed between -20°C and -50°C during cooling. During heating, aglass transition was observed between -50°C and 0°C. DSC-curve: Figure 2 (see attached document).The inflection point of the glass transition of the test substance was -19.38°C. An exothermic peak was observed from 175°C and 350°C. After the experiment, an orange residue remained in the sample container. The change of the colour indicated reaction and/or decomposition of the test substance.

Experiment 2: a lower heating rate was used. During cooling, a glass transition was observed between -20°C and -50°C. During heating, aglass transition between -50°C and 0°C was observed. The inflection point of the glass transition (melting point) of the test substance was now -21.80°C as a result of the lower heating rate. After the experiment, the sample appeared to be unchanged, i.e. no decomposition and/or evaporation were observed. Figure 3 (see attached document) shows the DSC-curve obtained.

Experiment 3: the experiment was performed to obtain a duplicate for the first experiment. The inflection point of the glass transition was -19.38°C. After the experiment, the sample appeared to be unchanged, i.e. no decomposition and/or evaporation were observed. DSC curve: Figure 4 (see attached document).

Experiment 4: performed according the OECD 113 guideline. An exothermic peak was observed between 175°C and 275°C. An endothermic peak was observed between 325°C and 400°C. DSC curve: see Figure 5. From this, it was concluded that no chemical reaction or transformation (other than melting) was observed at a temperature of < 150°C.

Applicant's summary and conclusion

Conclusions:

The melting temperature of the test substance is -19°C. Decomposition starts at 175°C.