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Administrative data

Endpoint:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
key study
Study period:
2008-09-16 till 2008-10-06
Reliability:
1 (reliable without restriction)
Cross-reference
Reason / purpose for cross-reference:
reference to same study

Data source

Reference
Reference Type:
study report
Title:
Unnamed
Year:
2009
Report date:
2009

Materials and methods

Test guidelineopen allclose all
Qualifier:
according to guideline
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Deviations:
no
Qualifier:
according to guideline
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
Deviations:
no
GLP compliance:
yes (incl. QA statement)
Type of method:
thermal analysis
Remarks:
for Preliminary Test and Main Test and capillary test for preliminary test

Test material

Reference
Name:
Unnamed
Type:
Constituent
Details on test material:
- Name of the test material (as cited in the study report: FAT 40842/A TE
- Substance type: coloring dye
- Physical state: solid, dark bluish green powder
- Analytical purity: 96%
- Lot/batch No.: Blau DRI 2098 Op 1/07
- Expiration date of the lot/batch: June 30, 2014
- Storage condition of test material: at room temperature at about 20 ºC

Results and discussion

Melting / freezing point
Melting / freezing pt.:
>= 214.6 - <= 214.7 °C
Atm. press.:
ca. 100 kPa
Decomposition:
yes
Decomp. temp.:
> 250 °C
Sublimation:
no

Any other information on results incl. tables

Melting Point / Melting Range

The capillary pre-test showed that the first peak observed in the DSC run not corresponds to the melting of the test item. In order to determine the melting more precisely, further DSC-runs were recorded between 150 °C and 250 °C with a heating rate of 5 °C/min. For the actual determination of the melting point, 3.70 mg and 3.91 mg, respectively, were heated up.

 

Heating[ºC]

 

Heating Rate [ºC]

Melting Point [ºC]

Melting Point [K]

Perliminary Test

25-400

20

217.4

490.6

Main Test Run 1

150 -250

5

214.7

487.9

Main Test Run 2

150 -250

5

214.6

487.8

Mean Melting Point

Standard deviation (±)

214.6

0.1

487.8

0.1

The study was performed under atmospheric pressure which was at that time ca. 100kPa. The exact value of the pressure was not recorded

Applicant's summary and conclusion

Conclusions:
The melting point of FAT 40842/A TE was determined to be 214.6 °C ± 0.1 °C which is equal
to 487.8 K ± 0.1 K by thermal analysis (DSC).
Executive summary:

Preliminary Tests

The DSC-curve of the preliminary test (heating rate of 20 °C/min from 25 °C to 400 °C) showed several endothermic heat effects. The first peak starting at 217.4 °C. After the experiment, the sample had lost about 19.36% of its mass and a black melt remained.

In order to define which of the endothermic heat effects corresponds to melting, a further pre-test was performed using the capillary tester. A total of 3 samples were heated up from 25 °C to 400 °C with a heating rate of 10 °C/min. At about 214 °C the test item started melting.

Main Tests Melting Point / Melting Range

In order to determine the melting more precisely, further DSC-runs were recorded between 150 °C and 250 °C with a heating rate of 5 °C/min. In the first main test run, the melting was observed at 214.7 °C, during the second main test run at 214.6 °C. During these runs, the sample lost no weight and a black melt remained.