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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:
2018-04-09 to 2018-09-12
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Reason / purpose for cross-reference:
reference to same 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, sealed container
Melting / freezing pt.:
>= 0 - <= 70 °C
Atm. press.:
991 hPa
Decomposition:
yes
Decomp. temp.:
>= 185 °C

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

In both DSC runs endothermic effects were observed in the temperature ranges from 0 °C to 70 °C, from 260 °C to 400 °C, from 460 °C to 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]

PN15432

8.17

39.20
261.32
487.08

0 – 70 (endo)
260 – 370 (endo)
460 – 580 (endo)

6.92 mg
85 %

990.8

PN15433

11.37

38.28
274.63
499.52

10 – 70 (endo)
270 – 400 (endo)
480 – 600 (endo)

9.91 mg
87 %

990.8

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. The liquefaction of the test item was observed at approx. 15 °C and at approx. 185 °C small bubbles started to form and to rise in the test glass. The temperature of the test glass was not increased further.

Thermal stability (DSC)

No significant exothermic or endothermic effects were observed up to 450 °C. At 450 °C the DSC signal showed a high noise so that the thermograms above this temperatures cannot be interpreted without doubt.

Results of the DSC-measurements

No.

Sample weight [mg]

Start of effect [°C]

Energy* [J/g]

PN15430

9.68

-

-

PN15431

11.85

-

-

* Positive energy for endothermic processes

Conclusions:
Melting and Boiling Point:
In the differential scanning calorimetry measurements according to Regulation EC No. 440/2008 Method A.1./A.2 and OECD Test Guidelines 102/103 (1995) at atmospheric pressure (991 hPa) endothermic effects were observed in the temperature ranges from 0 °C through 70 °C, from 260 °C through 400 °C, from 460 °C through 600 °C, but no exothermic effects were observed.
The visual observation of the test item being heated in a test glass showed that the test item starts to liquefy at approx. 15 °C and that small bubbles started to form and to rise in the test glass at approx. 185 °C.
Based on the results and observations, it may be assumed that the test item has a melting range between 0 and 70 °C and decomposes before boiling at temperatures ≥ 185 °C.

Thermal Stability:
The test item showed no significant endothermic or exothermic effects up to a temperature of 450 °C in the differential scanning calorimetry measurements according to OECD Test Guideline 113 (1981). The DSC signal at temperatures exceeding 450 °C does not allow the definite interpretation of the thermograms above this temperature.

Description of key information

The test item starts melting between 0 and 70 °C and decomposes before boiling at temperatures ≥ 185 °C.

Key value for chemical safety assessment

Additional information

Melting and Boiling Point:

In thedifferential scanning calorimetry measurements according to Regulation EC No. 440/2008 Method A.1./A.2 and OECD Test Guidelines 102/103 (1995) at atmospheric pressure (991 hPa) endothermic effects were observed in the temperature ranges from 0 °C through 70 °C, from 260 °C through 400 °C, from 460 °C through 600 °C, but no exothermic effects were observed.

The visual observation of the test item being heated in a test glassshowed that the test item starts to liquefy at approx. 15 °C and that small bubbles started to form and to rise in the test glass at approx. 185 °C.

Based on the results and observations, it may be assumed that the test item has a melting range between 0 and 70 °C and decomposes before boiling at temperatures ≥ 185 °C.

Thermal Stability:

The test item showed no significant endothermic or exothermic effects up to a temperature of 450 °C in the differential scanning calorimetry measurements according to OECD Test Guideline 113 (1981). The DSC signal at temperatures exceeding 450 °C does not allow the definite interpretation of the thermograms above this temperature.

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