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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:
2018-03-14 to 2018-05-07
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:
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:
other: Thermal Stability (OECD 113)
Version / remarks:
1981
Deviations:
no
GLP compliance:
yes (incl. QA statement)
Remarks:
signed 2017-02-28
Type of method:
differential scanning calorimetry
Specific details on test material used for the study:
Storage Conditions: Room temperature, tightly closed container, dry
Decomposition:
yes
Decomp. temp.:
ca. 230 °C
Remarks on result:
other: no distinct phase transitions, melting and boiling can be derived

Melting and Boiling Point (DSC and Measurement in Test Glass)

In both DSC runs endothermic effects were observed in the temperature ranges from -20 °C through 40 °C, from 70 °C through 180 °C, from 250 °C through 330 °C and from 360 °C through 600 °C. In both DSC runs no exothermic effect was detected.

Results of the DSC-measurements

No.

Sample weight [mg]

Onset of Effect
[°C]

Range of effect
[°C]

Weight loss

Atmospheric pressure [hPa]

PN15501

6.23

-7.52
95.04
265.58
380.20

-20 – 40 (endo)
80 – 180 (endo)
250 – 330 (endo)
360 – 600 (endo)

5.36 mg
86 %

1012.5

PN15506

4.78

-14.23
80.96
259.04
382.65

-20 – 40 (endo)
70 – 180 (endo)
260 – 280 (endo)
380 – 510 (endo)

4.06 mg
85 %

1016.2

It is not possible to assign any of the observed endothermic effects definitely to melting or boiling of the test item.

For verification of the DSC results the test item was additionally tested in a test glass. At approx. 60 °C the test item started to soften but did not melt. At approx. 230 °C the colour of the test item changed to brown while small bubbles started to form.

Thermal stability (DSC)

An exothermic effect was observed starting from 140 °C with an energy release of >-80 J/g.

Results of the DSC-measurements

No.

Sample weight [mg]

Start of effect [°C]

Energy* [J/g]

PN15504

5.58

140

-80 (exothermic)

PN15509

5.38

140

-60 (exothermic)

*Negative energy for exothermic processes

Conclusions:
Melting and Boiling Point:
Neither a melting nor a boiling of the test item could be definitely observed by differential scanning calorimetry according to Regulation EC No. 440/2008 Methods A.1./A.2 and OECD Test Guidelines 102/103 (1995) at atmospheric pressure (1012 hPa to 1016 hPa). The visual observation of the test item being heated in a test glass suggests that the test item softens but does not melt at approx. 60 °C and that it decomposes under gas formation at approx. 230 °C.
Based on the results and observations no distinct phase transitions, melting and boiling can be derived for the test item. A mass loss of ~86 % was observed.

Thermal Stability:
The test item showed an exothermic effect at 140 °C with an energy release of -80 J/g as observed in the differential scanning calorimetry measurements according to OECD Test Guideline 113 (1981).

Description of key information

Based on the DSC results and visual observations no distinct phase transitions, melting and boiling can be derived for the test item.

Key value for chemical safety assessment

Additional information

Melting and Boiling Point:

Neither a melting nor a boiling of the test item could be definitely observed by differential scanning calorimetry according to Regulation EC No. 440/2008 Methods A.1./A.2 and OECD Test Guidelines 102/103 (1995) at atmospheric pressure (1012 hPa to 1016 hPa).

The visual observation of the test item being heated in a test glass suggests that the test item softens but does not melt at ~60 °C and that it decomposes under gas formation at ~230 °C.

Based on the results and observations no distinct phase transitions, melting and boiling can be derived for the test item. A mass loss of ~86 % was observed.

Thermal Stability:

The test item showed an exothermic effect at 140 °C with an energy release of -80 J/g as observed in the differential scanning calorimetry measurements according to OECD Test Guideline 113 (1981).