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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:
2018-04-09 to 2018-09-14
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.:
>= -40 - <= -10 °C
Decomposition:
yes
Decomp. temp.:
>= 100 °C
Remarks on result:
other: the test item decomposes while boiling

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

In both DSC runs endothermic effects were observed in the temperature ranges from -40 °C through -20 °C, from 180 °C through 270 °C and from 460 °C through 590 °C. A mass loss of ~85 % was observed.

Results of the DSC-measurements

No.

Sample weight [mg]

Onset of Effect [°C]

Range of effect [°C]

Weight loss

Atmospheric pressure [hPa]

PN15517

21.43

-37.31
217.98
527.37

-40 – -20 (endo)
180 – 260 (endo)
470 – 590 (endo)

18.46 mg
86 %

1012.1

PN15531

8.57

-72.62
212.89
500.28

-40 – 20 (endo)
180 – 270 (endo)
460 – 580 (endo)

7.30 mg
85 %

1002.1

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. -10 °C the test item started to liquefy. At approx. 100 °C small bubbles started to form and to rise in the test glass. Then the test was aborted.

Note that the results of the DSC measurements and of the measurements in the test glass are not in accordance with each other.

Thermal stability (DSC)

Two endothermic effects starting at approx. 150 °C - 190 °C and at 210 °C were observed. Around 340 °C the DSC signal showed a high noise so that the thermograms above this temperatures cannot be interpreted without doubt.

It can be estimated that the test item decomposes at approx. 200 °C.

Results of the DSC-measurements

No.

Sample weight [mg]

Start of effect [°C]

Energy* [J/g]

PN15518

6.25

150
210

30 (endothermic)
90 (endothermic)

PN15420

8.88

190
210

10 (endothermic)
80 (endothermic)

* 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 -40 °C through -20 °C, from 180 °C through 270 °C and from 460 °C through 580 °C. A mass loss of ~85 % was observed.
The visual observation of the test item being heated in a test glass gave that the test item starts to liquefy at approx. -10 °C and that small bubbles started to form and to rise in the test glass at approx. 100 °C.
Based on the results and observations, it may be assumed that the test item liquefies between -40 and -10 °C and decomposes while boiling at temperatures ≥ 100 °C.

Thermal Stability:
The test item showed two endothermic effects, but no exothermic effects up to a temperature of 340 °C in the differential scanning calorimetry measurements according to OECD Test Guideline 113 (1981). The first endothermic effect started at 150 °C, 190 °C resp. and the second at 210 °C. The DSC signal showed a high noise above 340 °C so that the thermograms above this temperature cannot be interpreted without doubt.

Description of key information

Based on the results and observations, it may be assumed that the test item liquefies between -40 and -10 °C and decomposes while boiling at temperatures ≥ 100 °C.

Key value for chemical safety assessment

Additional information

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 -40 °C through -20 °C, from 180 °C through 270 °C and from 460 °C through 580 °C. A mass loss of ~85 % was observed.

The visual observation of the test item being heated in a test glass gave that the test item starts to liquefy at approx. -10 °C and that small bubbles started to form and to rise in the test glass at approx. 100 °C.

Based on the results and observations, it may be assumed that the test item liquefies between -40 and -10 °C and decomposes while boiling at temperatures≥100 °C.

 

Thermal Stability:

The test item showed two endothermic effects, but no exothermic effects up to a temperature of 340 °C in the differential scanning calorimetry measurements according to OECD Test Guideline 113 (1981). The first endothermic effect started at 150 °C, 190 °C resp. and the second at 210 °C. The DSC signal showed a high noise above 340 °C so that the thermograms above this temperature cannot be interpreted without doubt.