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Melting point / freezing point

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Reference
Endpoint:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
key study
Study period:
18 April - 09 August, 2017
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Qualifier:
according to guideline
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Version / remarks:
July 27, 1995
Deviations:
no
Qualifier:
according to guideline
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
Version / remarks:
31 May 2008
Deviations:
no
Qualifier:
according to guideline
Guideline:
EPA OPPTS 830.7200 (Melting Point / Melting Range)
Version / remarks:
March, 1998
Deviations:
no
GLP compliance:
yes (incl. QA statement)
Type of method:
differential scanning calorimetry
Specific details on test material used for the study:
Expiry date 16 June 2020
Key result
Melting / freezing pt.:
>= 267 - <= 276 °C
Remarks on result:
other: Not the whole sample was melted. Using a 10 °C/min heating rate, the melting point of a small part of Brown 3 was determined to be in the range of 267 - 276 °C (540 - 550 K), but the melting point of the whole test item was not observed up to 500 °C
Key result
Melting / freezing pt.:
> 500 °C
Remarks on result:
other: The melting point of the whole test item was not observed up to 500 °C.

Values of the DSC run in the first experiment

Sample weight [mg]

Loss of Mass of the Sample (%)

Onset of effect [°C]

Endset of effect [°C]

Peak Maxium [°C]

Energy [J/g]

8.73

31

266.66

276.20

272.70

- 18.37 (endothermic)

Values of the DSC run in the second experiment

Sample weight [mg]

Loss of Mass of the Sample (%)

Onset of effect [°C]

Endset of effect [°C]

Peak Maxium [°C]

Energy [J/g]

9.40

29

266.48

276.58

272.89

- 15.37 (endothermic)

Summary of the DSC Test of Test Item

 

Experiment 1

Experiment 2

Mean

Onset of effect [°C]

267

266

267

Endset of effect [°C]

276

277

276

Values of the DSC run in the Confirmatory test

Sample weight [mg]

Loss of Mass of the Sample (%)

Onset of effect [°C]

Endset of effect [°C]

Peak Maxium [°C]

Energy [J/g]

4.43

23

264.15

273.94

270.39

- 16.86 (endothermic)


Conclusions:
The test was carried out at normal atmospheric pressure. Based on the thermograms and the unchanged appearance of test item after the tests, it is concluded that not the whole sample was melted, only a small part of it. Using a 10 °C/min heating rate, the melting point of a small part of Brown 3 was determined to be in the range of 267 - 276 °C (540 - 550 K), but the melting point of the whole test item was not observed up to 500 °C.
Executive summary:

For the determination of the melting point or melting range, differential scanning calorimetry method was used. A small amount of the test item was inserted into the furnace of the device and the melting point was determined based on measuring the heat flow while raising the temperature. The heat flow in and out of a sample and a reference sample was measured as a function of temperature as the sample was heated.

When the sample undergoes a phase transition, the corresponding change of enthalpy gives a departure from the base line of the heat flow record. The difference in energy input necessary to maintainidenticaltemperatures between the substance and the reference sample is recorded. The measurement signal is the energy absorbed by or released by the sample.

The test was carried out at normal atmospheric pressure. Based on the thermograms and the unchanged appearance of test item after the tests it is concluded that not the whole sample melted, only a small part of it. Using a 10 °C/min heating rate, the melting point of a small part of Brown 3was determined to be in the range of 267 - 276 °C (540 - 550 K), but themelting point of the whole test item was not observed up to 500 °C.

 

Description of key information

The test was carried out at normal atmospheric pressure. Using a linear heating rate melting point was not observed from room temperature up to 500 °C

Key value for chemical safety assessment

Additional information