Registration Dossier

Administrative data

Endpoint:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
key study
Study period:
8 January 2018 - 29 November 2018
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study

Data source

Reference
Reference Type:
study report
Title:
Unnamed
Year:
2018
Report Date:
2019

Materials and methods

Test guidelineopen allclose all
Qualifier:
according to
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Deviations:
no
Qualifier:
according to
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
Deviations:
no
Qualifier:
according to
Guideline:
EPA OPPTS 830.7200 (Melting Point / Melting Range)
Deviations:
no
GLP compliance:
yes (incl. certificate)
Type of method:
differential scanning calorimetry

Test material

Reference
Name:
Unnamed
Type:
Constituent
Test material form:
solid
Details on test material:
- Physical state: powder/solid
- Appearance: white powder
Specific details on test material used for the study:
- Batch n°: 397451
- Expiration date: 07 July 2018
- Purity: 99.86 %
- Storage condition of test material: In refrigerator (2-8°C)

Results and discussion

Melting / freezing point
Key result
Melting / freezing pt.:
28.2 °C
Atm. press.:
1 013.25 hPa
Decomposition:
no
Remarks on result:
other: A colourless molten residue remained after the preliminary and main tests to determine the melting temperature

Any other information on results incl. tables

Preliminary test

From the TGA curve it could be derived that the weight of the sample decreased significantly starting at 150°C. At 197°C the sample weight has decreased by 25%. After the experiment, a colourless molten residue remained in the sample container (original colour: white).

Main tests

In order to determine the melting more precisely, the DSC curve with a heating rate of 20°C/min was obtained and showed an endothermic peak between 0°C and 50°C. The extrapolated onset temperature of the peak was 28.172°C. The endothermic effect was most likely obtained due melting of the test item. A second endothermic peak was observed starting at 150°C. After the experiment, a colourless molten residue remained in the sample container (original colour: white).

To investigate the melting peak, Experiment 2 was stopped directly after the melting peak. The extrapolated onset temperature of the melting peak was 28.393°C. After the experiment, a colourless molten residue remained in the sample container which demonstrated that melting was the reason for the endothermic effect.

In order to investigate the second endothermic peak, Experiment 3 was stopped at a higher temperature. The extrapolated onset temperature of the melting peak was 28.061°C. An endothermic peak was observed between 50°C and 125°C. The endothermic effect was most likely obtained due to evaporation of moisture. Another endothermic peak was observed between 150°C and 250°C and the extrapolated onset temperature was 219.934°C. After the experiment it was observed that the test item had evaporated from the sample container. The second endothermic effect was most likely obtained due to boiling of the test item.

The last experiment (performed as duplicate determination of the boiling point) showed similar results as Experiment 1. The extrapolated onset of the melting peak was 28.026°C. The extrapolated onset of the boiling peak was 219.909°C. After the experiment it was observed that the test item had evaporated from the sample container.

Applicant's summary and conclusion

Conclusions:
The melting temperature of 1,4-dioxan-2-one (PDO monomer) was determined at 28.2°C (301.3K) by using DSC.