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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:
07 Jun 2018 to 12 Sep 2018
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Qualifier:
according to guideline
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Version / remarks:
27 July 1995
Deviations:
no
Qualifier:
according to guideline
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
Version / remarks:
30 May 2008
Deviations:
no
GLP compliance:
yes (incl. QA statement)
Type of method:
differential scanning calorimetry
Remarks:
visual method (metal block) as supporting information
Key result
Melting / freezing pt.:
>= 133 - <= 146 °C
Atm. press.:
100.8 kPa
Decomposition:
yes
Decomp. temp.:
ca. 293 °C

Tables: Thermographic data of the preliminary screening and determinations 1 – 4.

  

Thermal Event

Interpretation

Temperature

Determination A

Determination B

ºC

K

ºC

K

Endotherm (onset)

Loss of volatiles

90.5

363.6

90.5

363.7

Endotherm (onset)

Melting

140.5

413.6

141.5

414.7

Endotherm (left limit)

Decomposition with boiling

294.6

567.8

294.1

567.2

  After heating to 450 °C, the crucible had lost an average of 97% of the original mass.

Thermal Event

Interpretation

Temperature

Determination 1

Determination 2

ºC

K

ºC

K

Endotherm (onset)

Loss of volatiles

91.4

364.6

91.2

364.4

Endotherm (onset)

Melting

141.7

414.8

141.0

414.1

Endotherm (left limit)

Decomposition with boiling

293.9

567.0

293.0

566.2

Atmospheric pressure: 100.8 kPa

After heating to 450 °C, the crucibles had lost an average of 95% of their original mass. The residue in the crucible was observed to be a black solid around the periphery.

Decomposition with boiling from approximately 293 ºC (566 K) at 100.8 kPa.

Thermal Event

Interpretation

Temperature

Determination 3

Determination 4

ºC

K

ºC

K

Endotherm (onset)

Loss of volatiles

90.9

364.1

91.1

364.3

Endotherm (onset)

Loss of volatiles

127.5

400.7

127.5

400.7

Endotherm

Melting range

133.1 to 145.7

406.3 to 418.8

133.1 to 145.4

406.3 to 418.6

After heating to 200 °C, the crucibles had not lost mass.

The residue in the crucibles were observed to be off white brittle solid around the periphery.

Melting range: 133 to 146 ºC (406 to 419 K)

 

DISCUSSION

The melting determinations demonstrated three endotherms. The first and second were considered to be possibly due to loss of volatile constituent. The third broad endotherm was considered to be due to the melting phase transition of the test item. The shallow exotherm (not integrated) after melting up to approximately 170 °C may be due to further reaction or decomposition in the liquid state. The visual assessment confirmed the interpretation of the DSC determinations. Similar thermograms were obtained under air (preliminary/screen determinations) and nitrogen atmospheres (determinations 1 and 2) indicating the decomposition was most likely to be thermal rather than oxidative.

Conclusions:
The test item was determined to melt in the range of 133 to 146 ºC (406 to 419 K).
Executive summary:

The study using the differential scanning calorimetry, using a procedure designed to be compatible with OECD TG 102, was performed to determine the melting temperature of the test item in compliance with GLP. The test item was observed to melt in the range of 133 to 146 ºC (406 to 419 K).

Description of key information

melting point in the range of 133 to 146 ºC, decomposition temperature from approximately 293 °C, equivalent to OECD 102, differential scanning calorimentry, Butler 2018

Key value for chemical safety assessment

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

Additional information