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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 guidelineopen allclose all
Qualifier:
according to guideline
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
Version / remarks:
(2008)
Deviations:
no
Qualifier:
according to guideline
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Version / remarks:
(1995)
Deviations:
no
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

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 pointopen allclose all
Melting / freezing pt.:
-19 °C
Remarks on result:
other: glass transition
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.