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Melting point / freezing point

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Endpoint:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
key study
Study period:
The experimental phase was undertaken between 29.09.1995 and 07.12.1995
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Qualifier:
according to guideline
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
Deviations:
no
GLP compliance:
yes
Type of method:
capillary method
Melting / freezing pt.:
>= 251 - <= 252.5 °C
Atm. press.:
ca. 1 013 hPa

The colour changed at 238 °C.

Endpoint:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
key study
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
comparable to guideline study
Principles of method if other than guideline:
Differential scanning calorimetry method is used.
GLP compliance:
no
Type of method:
differential scanning calorimetry
Melting / freezing pt.:
>= 252.16 - <= 252.73 °C
Atm. press.:
ca. 1 002.3 mBar
Decomposition:
no

Pre-test following Siwoloboff

Observations

Temperatures in °C

Melting process

Since 250

Yellow turbid liquid, opaque. Getting slightly darker, not homogeneous, seems to be two phasis

260

Bubbles on the surface

283

Strong boiling visible on the surface, heating switched off.

Substance is reddish-brown and turbid

289.6

 

After cooling down the test substance solidified as brown mass, on the top darker.

 

Security Pre-test for the DSC instrument

The crucible was visually unchanged after reaching a temperature of 300 °C and after reaching the temperature of 400 °C around the perforation the test substance exited. After reaching the temperature of 450 °C no further changes were observed, the exited test substance was turbid and pale brown. The weight was recorded with 45.97 mg.

 

The DSC measurement of indium after calibration met the validity criteria.

 

Result

Temperature [°C]

Energy [J/g] / Heat flow [mW]

Melting Point (onset)

252.55 (first determination)

252.16 (second determination)

252.73 (third determination)

108.02

104.14

114.12

 

Two endothermic events were detected.

 

The first event is stated as the melting point and is given in range of:

 

252.16 °C to 252.73 °C (525.31K to 525.88 K).

Description of key information

251-252 .73°C (EU A.1, capillary method and DSC method)

Key value for chemical safety assessment

Additional information