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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:
10.-14.07.2017
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
Remarks:
and capillary method
Key result
Melting / freezing pt.:
>= 141 - <= 150 °C
Atm. press.:
1 013 hPa
Decomposition:
no

DSC measurement

Two DSC measurements with a heating rate of 10 K/min showed two endothermal effects (melting) in the temperature range of 105 - 120 °C and 140 - 160 °C The first measurement showed a drift of the base line starting at 460 °C. This is possibly due to a decomposition of the sample since after the measurement a beige residue was observed in the crucible. The onset temperatures (see Table 1) were derived from the intersection of the tangent line with the highest slope of the endothermal peak with the baseline.

Table 1: Melting point (DSC measurements)

Ident No.

Test item / mg

Starting temperature /

°C

Final test temperature /

°C

Temperature range (endothermal) /

°C

Onset (melting) / °C

Crucible

Observations after the measurement

36368

9.94

25

500

105-120

140-160

109.2

144.6

Aluminium with a hole

Measurement continued after melting, beige residue after measurement

36370

11.13

25

200

105-120

140-155

107.7

145.4

Aluminium with a hole

solidified melt after the measurement

 

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.

Table 2: Results of the capillary method

 

No.

Set point / °C

Heating rate / K/min

End point / °C

Remarks

1

80

10

170

Approx. 141 °C:

Approx. 150 °C:

Approx. 170 °C:

test item started to melt

test item completely melted

no further change observed

 

Conclusions:
The melting point of the test substance is in the range of 141 -150°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 and capillary method. The test item and the reference were heated up from the starting temperature to the final temperature at a constant heating rate in a defined atmosphere (nitrogen). Aluminium crucibles with hole were used as containers for the test item and the reference. The test item showed two endothermal effects. The first was observed with an onset temperature of 108 - 109 °C in the DSC-measurement (optical observation: no effect was observed). The second effect was observed with an onset temperature of 145 °C in the DSC-measurement (optical observation: start of melting at 141 °C, completely melted at 150 °C). The test item had a melting point in the range of 141 -150 °C (1013 hPa).

Description of key information

The test item had a melting point in the range of 141 - 150 °C (reference 4.2-1).

Key value for chemical safety assessment

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 and capillary method. The test item and the reference were heated up from the starting temperature to the final temperature at a constant heating rate in a defined atmosphere (nitrogen). Aluminium crucibles with hole were used as containers for the test item and the reference. The test item showed two endothermal effects. The first was observed with an onset temperature of 108 - 109 °C in the DSC-measurement (optical observation: no effect was observed). The second effect was observed with an onset temperature of 145 °C in the DSC-measurement (optical observation: start of melting at 141 °C, completely melted at 150 °C). The test item had a melting point in the range of 141 -150 °C (1013 hPa).