Registration Dossier

Administrative data

Endpoint:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
key study
Study period:
19 Sep 2017 - 24 Nov 2017
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 guidelineopen allclose all
Qualifier:
according to
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
Version / remarks:
2008
Deviations:
no
Qualifier:
according to
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Version / remarks:
1995
Deviations:
no
Qualifier:
according to
Guideline:
EPA OPPTS 830.7200 (Melting Point / Melting Range)
Version / remarks:
1998
Deviations:
no
Principles of method if other than guideline:
DSC experiments were performed according to the above mentioned guidelines. No melting/freezing point could be determined by DSC. Therefore an additional experiment was performed in which the consistency of the substance was determined by visual observation after storage in freezers at ca. -20°C and at ca. -80°C. The additional experiment is not a guideline study but was described in sufficient detail.
GLP compliance:
yes
Type of method:
other: 'differential scanning calorimetry' and 'visual observation after storage in freezer'

Test material

Reference
Name:
Unnamed
Type:
Constituent

Results and discussion

Melting / freezing point
Key result
Decomposition:
yes
Decomp. temp.:
ca. 200 °C
Remarks on result:
other: Glass transition point: -53.7°C. No melting/freezing point was determined between 25°C and -90°C.

Any other information on results incl. tables

TGA EXPERIMENT (PRELIMINARY TEST)

Significant decrease of weight from 100°C. 25% weight loss at 361°C and 70% at 467°C.

After the experiment, a black molten residue remained in the sample container (original colour: amber) and a black residue was observed on the lid of the sample container.

DSC EXPERIMENT 1

During cooling a glass transition was observed between -40°C and -70°C and an exothermic peak was observed between 0°C and -40°C. The exothermic effect was most probably obtained by

crystallisation of one or more components of the test item. During heating a glass transition was observed between -75°C and -25°C (inflection point: -53.666°C).

A small endothermic peak was observed between -25°C and 25°C and subsequently an endothermic peak was observed between 100°C and 175°C followed by a strong exothermic effect starting at 200°C.

After the experiment, a black residue remained in the sample container. This colour change indicated degradation and/or decomposition of the test item. 

DSC EXPERIMENT 2

DSC experiment 2 was not considered valid due to a technical malfunction.

DSC EXPERIMENT 3

During heating an endothermic signal between 60 and 150°C similar to Experiment 1 was obtained. 

During cooling no crystallisation was observed. 

During the second heating no melting or evaporation was observed. This demonstrated that the two endothermic signals during heating in Experiment 1 derived from melting and evaporation of a component of the test item. As significant weight loss of the test item was observed in TGA analysis only at temperatures higher than 150°C, these effects were considered not representative for the (overall) test item. 

After the experiment, a black residue remained in the sample container. 

STORAGE IN FREEZER TEST

It was observed after storage that the test item was a viscous liquid (≤ -15°C freezer) and a sticky solid (≤ -80°C freezer). 

DATA HANDLING

The glass transition temperature was determined as the glass transition temperature of Experiment 1 (-53.666°C).

Applicant's summary and conclusion

Conclusions:
The substance has no melting point. A glass transition temperature of -53.7°C was determined.
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 experiments showed no effect due to freezing of the substance between 25°C and -90°C. A glass transition temperature of -53.7°C was determined. During DSC and TGA experiments reaction and/or decomposition of the substance was observed at >200°C. After storage in freezers, the substance was visually observed to be a viscous liquid (≤ -15°C freezer) and a sticky solid (≤ -80°C freezer). Based on all results it was concluded that the substance has no melting point.

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