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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:

Experiment start date - 22 March 2010; Experiment completion date - 23 March 2010; Study completion date - 31 May 2010.

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Qualifier:

according to guideline

Guideline:

EU Method A.1 (Melting / Freezing Temperature)

Deviations:

no

Qualifier:

according to guideline

Guideline:

OECD Guideline 102 (Melting point / Melting Range)

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Type of method:

thermal analysis

Specific details on test material used for the study:

Identification: FAT 40851/A TE
Batch Number: TZ 5891 / BOP 02-09
Purity: 69.9 % all coloured components
Appearance: Orange powder
Expiry Date: July 31, 2014
Storage Conditions: At room temperature at about 20 °C

Melting / freezing pt.:

> 400 °C

Atm. press.:

1 atm

Decomposition:

ambiguous

Sublimation:

no

Preliminary Test

The DSC-curve of the preliminary test (heating rate of 20 °C/min from 25 °C to 400 °C). An endothermic heat effect was observed starting at 64.9 °C. After the experiment, the sample had lost about 17 % of its mass and the sample was a dark powder.

 

Main Test

In order to investigate the endothermic heat effect more precisely, a further DSC-run was recorded between 25 °C and 230 °C with a heating rate of 10 °C/min. The endothermic heat effect starting at 91.2 °C was not due to melting, as the test item was still a powder after the test. The loss of 8.7 % of its mass during this run might be the result of emitting water.

Conclusions:

Using thermal analysis (DSC) no melting could be observed for test substance in the temperature range between 25 °C to 400 °C.

Executive summary:

The determination of the melting point/melting range of the test item was performed under GLP according to the EEC Directive 92/69 and Council Regulation (EC) No. 440/2008, A.1 “Melting/Freezing temperature“ and to the OECD Guideline No. 102: “Melting point / melting range“, adopted July 27, 1995. A test item amount of 4.89 mg was heated up from 25 °C to 400 °C at a rate of 20 °C/min. The quantities of heat absorbed or released were measured and recorded. Before and after the test, the weight and the appearance of the sample were determined. The DSC-curve of this preliminary test (heating rate of 20 °C/min from 25 °C to 400 °C). An endothermic heat effect was observed starting at 64.9 °C. After the experiment, the sample had lost about 17 % of its mass and the sample was a dark powder. In order to investigate the endothermic heat effect more precisely, a further DSC-run was recorded between 25 °C and 230 °C with a heating rate of 10 °C/min. 5.43 mg of the test item were heated up from 25 °C to 230 °C. The endothermic heat effect starting at 91.2 °C was not due to melting, as the test item was still a powder after the test. The loss of 8.7 % of its mass during this run might be the result of emitting water. Thus, no melting could be observed for test substance in the temperature range between 25 °C to 400 °C.

Description of key information

The substance has a melting point >400 °C.

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:

400 °C

Additional information

The melting point of the test item FAT 40851/A was tested in valid GLP study in accordance with EU Method A.1. To this end, approximately 5 mg test item was heated from 25 to 400 °C in steps of 20 °C/minute in a thermal analysis (DSC). An endothermic heat effect was seen in the experiment, which was not due to melting. No melting of the substance was observed up to the maximum temperature of 400 °C.