Registration Dossier

Administrative data

Endpoint:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
key study
Study period:
14 February 2018 to 14 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
Report Date:
2018

Materials and methods

Test guideline
Qualifier:
according to
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Version / remarks:
27 July 1995
Deviations:
no
GLP compliance:
yes (incl. certificate)
Other quality assurance:
ISO/IEC 17025 (General requirements for the competence of testing and calibration laboratories)
Type of method:
differential scanning calorimetry

Test material

Reference
Name:
Unnamed
Test material form:
liquid
Details on test material:
Appearance: Straw to yellow syrup
Purity/Composition: Not indicated
Test item storage: At room temperature

Additional information
Test Facility test item number: 209099/A
Purity/Composition correction factor: No correction factor required
Test item handling: No specific handling conditions required
Specific details on test material used for the study:
Appearance: Straw to yellow syrup
Purity/Composition: Not indicated
Test item storage: At room temperature

Additional information
Test Facility test item number: 209099/A
Purity/Composition correction factor: No correction factor required
Test item handling: No specific handling conditions required

Results and discussion

Melting / freezing point
Key result
Melting / freezing pt.:
> 248.8 - < 305.9 K
Atm. press.:
ca. 1 013 hPa
Decomposition:
no
Sublimation:
no

Any other information on results incl. tables

Preliminary test 

The TGA curve of the test item is shown in Figure 1 (attached). Starting at 275°C, the weight of the sample decreased significantly. At 419°C, the sample weight had decreased by 25%.

After the experiment, a light yellow molten residue remained in the sample container (original colour: white) and a yellow residue was observed on the lid of the sample container. The change of the colour indicated reaction and/or decomposition of the test item.

Main study     

The DSC curve obtained with Experiment 1 is shown in Figure 2 (attached). During cooling, two exothermic peak between 20°C and -40°C were found (results are archived in the raw data). The effects were obtained due to crystallization of the test item. During heating multiple endothermic peaks were observed between -50°C and 75°C followed by an endothermic effect starting at 200°C. The extrapolated onset temperature of the first peak was -24.242°C and the peak maximum temperature of the third peak was 32.640°C. The endothermic effects were most likely obtained due to melting of the test item. The last endothermic effect was probably obtained due to reaction and/or decomposition of the test item.

After the experiment, a light yellow molten residue remained in the sample container (original colour: white). The change of the colour indicated reaction and/or decomposition of the test item. Based on this visual observation, it was found that the test item had molten and the change of the colour demonstrated reaction and/or decomposition of the test item.

In order to investigate the endothermic peaks, Experiment 2 was stopped directly after the third melting peak. Figure 3 (attached) shows the DSC curve obtained. The extrapolated onset temperature of the first peak was -24.316°C and the peak maximum temperature of the third peak was 32.941°C. After the experiment, a colourless molten residue remained in the sample container (original colour: white). It demonstrated that melting was the reason for the endothermic effects.

The melting temperature was determined as a melting range obtained from the average extrapolated onset of the first melting temperature (-24.3°C) and the average peak maximum of the last melting temperature (32.8°C).

Conclusion

The melting and boiling temperature of the test substance were determined by DSC.

The melting temperature ofthe test itemwas -24.3°C – 32.8°C (248.8K – 305.9K).

Reaction and/or decomposition of the test itemwas observed during DSC experiment at temperatures of > 200°C (> 423K). Boiling of the test item was not observed below the temperature at which reaction and/or decomposition started. Based on this, the test item has no boiling temperature.

Applicant's summary and conclusion

Conclusions:
The melting / freezing point of the test substance was found to be 248.8 to 305.9 K at 1013 hPa, under the conditions of the test.
Executive summary:

In this guideline (OECD 102) study, [conducted with GLP certification], the melting point of the test substance (EC 281-689-7) was found to be 248.8 to 305.9 K at 1013 hPa.