2-((E)-(4-((4-(1,3-dioxo-1,3-dihydro-2H-hetereocarbapolycyclo-2-yl)alkyl)(ethyl)amino)-2-methyl)diazenyl)-5-nitro-1,3-dicarbonitrile, polyphenyl

Melting point / freezing point

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 guideline

Test guideline 1

Qualifier:

according to guideline

Guideline:

OECD Guideline 102 (Melting point / Melting Range)

Deviations:

no

Test guideline 2

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.