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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:
September 08, 2021 - September 23, 2021
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Qualifier:
according to guideline
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
Version / remarks:
EC No. 440/2008
Deviations:
no
Qualifier:
according to guideline
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Version / remarks:
1995
Deviations:
no
GLP compliance:
yes (incl. QA statement)
Type of method:
differential scanning calorimetry
Remarks:
Additional measurement with the capillary method was performed in order to clarify the melting range.
Key result
Melting / freezing pt.:
>= 133 - <= 170 °C
Decomposition:
yes
Decomp. temp.:
>= 190 °C

Individual results:


Melting point / melting range: DSC measurement:


Two DSC measurements in aluminium crucibles with a hole showed a multistage endothermal effect in the temperature range of 90 – 200 °C with no clear melting point (onset). At 200 °C an exothermal effect started, indicating the decomposition of the test item.


The results of the DSC measurements are summarized in Table 1.


Table 1: Melting point (DSC measurements)




































Ident No.



Test item /


mg



Starting temperature /


°C



Final test temperature /


°C



Temperature range (endo-thermal) /


°C



Onset (melting) / °C



Crucible



Observations after the measurement



39741



12.61



25



500



90 –190



multi-stage



Aluminium with a hole



Black residue, mass loss 49 %



39744



12.65



25



200



95 – 195



multi-stage



Aluminium with a hole



Test item was a dark green melt



An additional measurement with the capillary method was performed in order to clarify the melting range.


Melting point / melting range: capillary tube in a metal block:


A measurement with the capillary method was performed to clarify the results of the DSC measurements. The filling height of the test item was approximately 5 mm.


The results are summarized in Table 2.


Table 2: Results of the capillary method


































No.






Set point /
°C



Heating rate / K/min



End
point /
°C



Remarks



1



120



1



200



136.7 °C: test item appeared wet


Approx. 160 °C: half of the test item appeared melted


169.7 °C: red melt


Approx. 190 °C: test item darkened to dark red



2



120



1



200



135.5 °C: test item started to melt


159.5 °C: half of the test item appeared melted


165.3 °C: red melt


Approx. 190 °C: test item darkened to dark red



3



120



1



200



133.3 °C: test item started to melt


155.3 °C: half of the test item appeared melted


163.9 °C: red melt


Approx. 190 °C: test item darkened to dark red



The capillary method measurement showed that the test item melted within a wide temperature range from 133 to 170 °C.


Under consideration of the results from the DSC measurements and the capillary method it was concluded that the test item melted within a range of 133 – 170 °C. Afterwards decomposition started.


The test item had a melting range of 133 – 170 °C.

Conclusions:
The test item Disperse Red 153 had a melting range of 133 - 170 °C.
Decomposition started at approximately 190°C.
Executive summary:

The melting point of the test item was measured by DSC-measurements and by capillary tubes in a metal block.


The test item Disperse Red 153 had a melting range according to European Commission Regulation (EC) No. 440/2008, A.1. as well as OECD 102 (1995) of 133 - 170 °C.

Description of key information

The melting point of the test item was measured by DSC-measurements and by capillary tubes in a metal block.


The test item Disperse Red 153 had a melting range according to European Commission Regulation (EC) No. 440/2008, A.1. as well as OECD 102 (1995) of 133 - 170 °C.

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:
133 °C

Additional information

The test item Disperse Red 153 had a melting range of 133 - 170 °C.


Decomposition started at approximately 190°C.