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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:
30 November 2016 - 16 August 2017
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Justification for type of information:
The study was conducted according to an internationally recognised method, and under GLP. The substance is considered to be adequately characterised. Therefore full validation applies.
Qualifier:
according to guideline
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Version / remarks:
1995
Deviations:
no
Qualifier:
according to guideline
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
Version / remarks:
2008
Deviations:
no
Qualifier:
according to guideline
Guideline:
EPA OPPTS 830.7200 (Melting Point / Melting Range)
Version / remarks:
1998
Deviations:
no
Principles of method if other than guideline:
Not applicable
GLP compliance:
yes (incl. QA statement)
Remarks:
UK GLP compliance programme (inspected on 05 July 2016 / signed on 28 Octobre 2016)
Type of method:
differential scanning calorimetry
Key result
Melting / freezing pt.:
ca. 188 °C
Atm. press.:
ca. 102 kPa
Decomposition:
yes
Remarks on result:
other: The test item was determined to decompose with softening/melting from approximately 188 °C (461 K) at 102 kPa.

Results

The thermograms and thermographic data for the determinations are shown in following figures and tables on the experimental report:

DSC Determination 1:

20 to 350°C at 20K/min

Atmospheric pressure: 103.3kPa

Crucible mass loss: 82%

Thermal events: endotherms at 38°C and at 180°C

DSC Determination 2:

20 to 350°C at 20K/min

Atmospheric pressure: 103.3 kPa

Crucible mass loss: 74%

Thermal events: endotherms at 35°C and at 180°C

DSC Determination 3 (under nitrogen):

20 to 350°C at 20K/min

Atmospheric pressure: 103.3 kPa

Crucible mass loss: 22%

Interpretation of determination 3: The thermogram profile is comparable to those of the tests performed under air and the appearance of the residue also indicates degradation of the test item. The degradation of the test item is therefore considered to be probably thermal and not oxidative.

DSC Determination 4 and 5:

20 to 140°C at 1K/min

Atmospheric pressure: 103.3 kPa

Crucible mass loss: 0%

Interpretation of determinations 4 and 5: The appearance of the residue indicates that the test item does not degrade or experience a phase transition below 140 ºC (413K).

DSC Determination 6:

20 to 100 °C at 1 °C/min,

100 to 20 °C at -1 °C/min,

20 to 100 °C at 1 °C/min

Atmospheric pressure : 98.8 kPa

Crucible mass loss : 0%

Interpretation of determination 6: This experiment indicates that the initial double endotherm cannot be attributed to the loss of a volatile component.

DSC Determination 7:

20 to 400 °C at 5 °C/min

Atmospheric pressure : 102.0 kPa

Crucible mass loss : 94%

DSC Determination 8:

20 to 400 °C at 5 °C/min

Atmospheric pressure : 102.0 kPa

Crucible mass loss : 94%

Interpretation of determinations 7 and 8: The first double endotherm, which cannot be attributed to a phase transition, degradation or the loss of a volatile component, starts from approximately 28 °C (301 K). The second endotherm, attributed to decomposition of the test item with softening/melting, starts from approximately 188 °C (461 K) at 102 kPa.

Discussion

The tests performed indicate that the appearance of the test item changed from a white powder to a yellow, orange and then light brown melted residue around the periphery of the crucible base as the temperature increased, suggesting that decomposition and softening/melting of the test item occurred. The weight loss recorded for the crucibles also indicated vaporization of the decomposition products at high temperatures.

Visual tests (metal block, liquid bath) were performed, but inconsistent temperature readings were obtained, so the observations were only used to aid with the interpretation of the thermograms. The final temperatures at which the thermal events occurred have therefore been taken from the DSC experiments, specifically from those performed at a heating rate of 5 °C/min, as this technique provides constant and reproducible heating of the samples.

The first endotherm/double endotherm from approximately 28 °C (301 K) at 102 kPa could not be attributed to a phase transition, degradation or the loss of a volatile component.

Conclusion

The test item was determined to decompose with softening/melting from approximately 188 °C (461 K) at 102 kPa.

Conclusions:
The test item was determined to decompose with softening/melting from approximately 188 °C (461 K) at 102 kPa.
Executive summary:

A GLP study was performed in order to determine the melting point of test item according OECD 102, resp. EU A.1 guideline, using the DSC method.

The tests performed indicate that the appearance of the test item changed from a white powder to a yellow, orange and then light brown melted residue around the periphery of the crucible base as the temperature increased, suggesting that decomposition and softening/melting of the test item occurred. The weight loss recorded for the crucibles also indicated vaporization of the decomposition products at high temperatures.

Visual tests (metal block, liquid bath) were performed, but inconsistent temperature readings were obtained, so the observations were only used to aid with the interpretation of the thermograms. The final temperatures at which the thermal events occurred have therefore been taken from the DSC experiments, specifically from those performed at a heating rate of 5 °C/min, as this technique provides constant and reproducible heating of the samples.

The first endotherm/double endotherm from approximately 28 °C (301 K) at 102 kPa could not be attributed to a phase transition, degradation or the loss of a volatile component.

Description of key information

The test item was determined to decompose with softening/melting from approximately 188 °C (461 K) at 102 kPa.

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:
188 °C

Additional information

Afully reliable experimental study, conducted according to OECD 102/ EU A1/OPPTS guideline is available.

It is considered as a key study, and the result is retained as key data.