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Physical & Chemical properties

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:
March 16, 2018 - May 29, 2018
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Qualifier:
according to
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Deviations:
no
Qualifier:
according to
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
Deviations:
no
GLP compliance:
no
Type of method:
differential scanning calorimetry
Key result
Melting / freezing pt.:
67.9 °C
Atm. press.:
1 013.25 hPa
Decomposition:
no
Sublimation:
no

Table 1: Results: Melting point / melting range: DSC measurement

Two DSC measurements with a heating rate of 10 K/min showed two endothermal effects in the temperature range of 60 - 90 °C. The onset temperature was derived from the intersection of the tangent line with the highest slope of the endothermal peak with the baseline.

 

Ident No.

 

Test item / mg

Starting temperature / °C

 

Final test temperature / °C

 
 

Temperature

range (endothermal)

/

°C

 

Onset

(melting) /

°C

 Crucible  

Observations

after the

measurement

 36879  16.19  25  500  60 - 90

  

67.59

(first

peak)

Aluminium

with a hole

 
 ----
 36881  10.78  25  120  65 - 90

  

67.84

(first

peak)

 

Aluminium

with a hole

Test item was

a solidified

melt

Mass loss:

5 %

 
 36882  16.55  25  500  70 - 90

  

67.70

(first

peak)

 

Aluminium

with a hole

 ---
 38026  10.49  25  75 68 - 75    68.52  

Aluminium

with a hole

 

Test item was

a solidified

melt

After the first three DSC-measurements an additional measurement with the capillary method was performed in order to clarify the melting point.

Table 2: 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. Since this measurement was performed only as a verifying screening a high heating rate of 10 K/min was chosen and therefore the absolute temperature values derived with the capillary method are not as accurate as the DSC results. The filling height of the test item was approximately 5 mm.

 No.  Set point/ °C  Heating rate/ K/min  End point /°C  Remarks
 1  50  10  100

Approx. 61 °C: test item started to melt

Approx. 64 °C: test item appeared melted, a short formation

of bubbles was observed

Conclusions:
The test item had a melting point of 67.9 °C.
Executive summary:

A study was conducted according to OECD TG 102 and Regulation (EC) No 440/2008 method A.1 to determine the melting point of the test item using differential scanning calorimetry. The test item was weighed into an aluminium crucible under an inert atmosphere (nitrogen). Open crucibles are used as containers for the test item and as empty reference crucible. The test item and the reference are heated up from the starting temperature to the final temperature at a constant heating rate in a defined atmosphere (nitrogen). The quantity of heat absorbed or released is measured and recorded. Two DSC measurements with a heating rate of 10 K/min showed two endothermal effects in the temperature range of 60 - 90 °C. A measurement with the capillary method was performed to clarify the results of the DSC measurements. Since this measurement was performed only as a verifying screening a high heating rate of 10 K/min was chosen and therefore the absolute temperature values derived with the capillary method are not as accurate as the DSC results. The filling height of the test item was approximately 5 mm. Under consideration of the results from the DSC measurements and the capillary method it was concluded that the test item melted at 67.9 °C. The second endothermal effect was accompanied by a mass loss of unknown origin. The formation of bubbles and the mass loss in the DSC measurement could have been caused by residual solvents within the wax-like test item. The test item had a melting point of 67.9 °C.

Description of key information

The test item had a melting point of 67.9 °C.

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:
67.9 °C

Additional information

A study was conducted according to OECD TG 102 and Regulation (EC) No 440/2008 method A.1 to determine the melting point of the test item using differential scanning calorimetry. The test item was weighed into an aluminium crucible under an inert atmosphere (nitrogen). Open crucibles are used as containers for the test item and as empty reference crucible. The test item and the reference are heated up from the starting temperature to the final temperature at a constant heating rate in a defined atmosphere (nitrogen). The quantity of heat absorbed or released is measured and recorded. Two DSC measurements with a heating rate of 10 K/min showed two endothermal effects in the temperature range of 60 - 90 °C. A measurement with the capillary method was performed to clarify the results of the DSC measurements. Since this measurement was performed only as a verifying screening a high heating rate of 10 K/min was chosen and therefore the absolute temperature values derived with the capillary method are not as accurate as the DSC results. The filling height of the test item was approximately 5 mm. Under consideration of the results from the DSC measurements and the capillary method it was concluded that the test item melted at 67.9 °C. The second endothermal effect was accompanied by a mass loss of unknown origin. The formation of bubbles and the mass loss in the DSC measurement could have been caused by residual solvents within the wax-like test item. The test item had a melting point of 67.9 °C (reference 4.2 -1).