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Melting point / freezing point

Link to relevant study record(s)

Reference

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

From 11 Aug 2020 to 17 Aug 2020

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Reason / purpose for cross-reference:

reference to same study

Qualifier:

according to guideline

Guideline:

EU Method A.1 (Melting / Freezing Temperature)

Version / remarks:

2016

Deviations:

no

Qualifier:

according to guideline

Guideline:

OECD Guideline 102 (Melting point / Melting Range)

Version / remarks:

1995

Deviations:

no

Qualifier:

according to guideline

Guideline:

EPA OPPTS 830.7200 (Melting Point / Melting Range)

Version / remarks:

1998

Deviations:

no

Principles of method if other than guideline:

An additional investigation of the melting temperature of the test item was performed by placing two subsamples of the test item for 18 hours at -22.2 ± 1.8°C and at -83.5 ± 1.6°C respectively.

GLP compliance:

yes

Type of method:

differential scanning calorimetry

Key result

Melting / freezing pt.:

> -90 - < 25 °C

Decomposition:

yes

Decomp. temp.:

ca. 200 °C

Remarks on result:

other: Multiple endothermic and crystallisation effects (DSC) between -90°C and 25°C but without a defined melting effect. The test item was observed to be a very viscous liquid, almost solid at ca. -22°C and a solid at ca. -83.5°C.

TGA RESULT

Starting at 250°C, the weight of the sample decreased significantly. At 336°C, the sample weight had decreased by 25%. After the experiment, a black charred residue remained in the sample container (original colour: black/brown). The change of the state of the test item indicated reaction and/or decomposition.

 

DSC RESULTS

Experiment 1 : During cooling multiple crystallisation and/or glass transition were observed (results are archived in the raw data). During heating multiple endothermic and crystallisation effects are observed between -90°C and 25°C. Between 50°C and 175°C endothermic effect was observed. The effect was most likely obtained due to the evaporation of impurities. Starting at 200°C an endothermic followed by an exothermic effect was observed. Based on the result of the pre-test, this effect was probably obtained due to reaction and/or decomposition of the test item. After the experiment, a black molten residue remained in the sample container (original colour: black/brown).

In order to investigate the endothermic effect starting at 200°C, a lower heating rate of 5°C/minute was applied in the Experiment 2. The value was similar to what was found in Experiment 1. The exothermic effect was significantly stronger. It demonstrated that reaction and/or decomposition of the test item was the reason for the exothermic effect. After the experiment, a black molten residue remained in the sample container.

 

STORAGE IN FREEZER FOLLOWED BY VISUAL OBSERVATION

It was observed after storage that the test item was a very viscous liquid, almost solid at -22.2 ± 1.8°C and a solid at -83.5 ± 1.6°C. 

Conclusions:

The melting temperature of the substance is between -90°C and 25°C. The substance has no boiling point.

Executive summary:

Differential Scanning Calorimetry was performed. The experiments were in accordance with EC A.1, OECD 102 and OPPTS 830.7200 (melting temperature). GLP-study.

Two DSC experiments were performed. Multiple endothermic and crystallisation effects were observed between -90°C and 25°C without a defined melting/freezing effect. An additional non-guideline experiment was performed in which samples were placed at ca. -20°C and ca. -80°C. The substance was observed to be a very viscous liquid, almost solid at ca. -22°C and a solid at ca. -84°C. Based on both DSC results and visual observation, the melting temperature of the test item was concluded to be between -90°C and 25°C.

Further heating in duplicate DSC experiments, resulted in endothermic and strong exothermic effects from 200°C onwards. Also significant weight loss from 250°C was noticed in a preliminary TGA experiment. Test sample appeared, after each DSC or TGA test, to be a black molten or charred residue. Overall, it was concluded that decomposition of the substance starts at ca. 200°C. Boiling of the substance was not observed below the decomposition temperature (i.e. at 200°C). The substance has no boiling point.

Description of key information

Differential Scanning Calorimetry (DSC) was performed in accordance with EC A.1, OECD 102 and OPPTS 830.7200 (melting temperature). Multiple endothermic and crystallisation effects were observed between -90°C and 25°C without a defined melting/freezing effect. Based on both DSC results and visual observation, the melting temperature of the test item was concluded to bebetween -90°C and 25°C.