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Melting point / freezing point

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Endpoint:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
weight of evidence
Study period:
2017-05-18 to 2017-07-26
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Qualifier:
according to
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Version / remarks:
adopted 27 July 1995
Deviations:
no
Qualifier:
according to
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
Version / remarks:
30 May 2008
Deviations:
no
GLP compliance:
yes (incl. certificate)
Type of method:
differential scanning calorimetry
Key result
Decomposition:
yes
Decomp. temp.:
>= 160 °C
Sublimation:
no
Remarks on result:
not determinable

A preliminary thermogravimetric measurement was performed over a temperature range from room temperature to approx. 600 °C.

Three steps were registered with maxima at 88 °C, 187 °C resp. 451 °C. A total mass loss of 46.7 % at the final temperature could be observed (mass change in the range until 110 °C: 0.9 %; mass change in the range from 110 to 280 °C: 3.2 %; mass change in the range from 280 to 600 °C: 42.1 %). Mass loss due to purging: 0.5%.

The DSC measurements were performed twice in the temperature range from 20 - 400 °C. To determine a possible boiling point more precisely a crucible lid with a hole of 50 µm diameter was used in the measurements to prevent evaporation.

No sharp endothermic peak indicating a melting point could be observed. ln the range of approx. 35 °C there was an indication for a glass transition.

Upon further heating the DSC-curve showed no endothermic peak. The course of the DSC-curve indicated decomposition starting at approx. 160 °C: Reweighing after the measurement showed that the sample had lost 6.7 %/ 7.1 % of its mass. After the first as well as after the second run the residue looked dark-brown discoloured and molten.

Conclusions:
The present study was performed according to OECD Test Guideline 102 (adopted 27 July, 1995) in order to determine the melting point of Compimide 183. A thermogravimetric measurement and subsequently a differential scanning calorimetry (DSC) was performed. In the course of the thermogravimetric curve three steps were registered with maxima at 88 °C, 187 °C resp. 451 °C. A total mass loss of 46.7 % at the final temperature could be observed (mass change in the range until 110 °C: 0.9 %; mass change in the range from 110 to 280 °C: 3.2 %; mass change in the range from 280 to 600 °C: 42.1 %). Mass loss due to purging: 0.5%. During the DSC no sharp endothermic peak indicating a melting point could be observed. In the range of approx. 35 °C there was an indication for a glass transition. Upon further heating the DSC-curve showed no endothermic peak. The course of the DSC-curve indicated decomposition starting at approx. 160 °C: Reweighing after the measurement showed that the sample had lost 6.7 %/ 7.1 % of its mass. Thus, Compimide 183 is considered to decompose but exhibits no melting or boiling point.
Endpoint:
melting point/freezing point
Remarks:
results were obtained from a study according to OECD 104
Type of information:
experimental study
Adequacy of study:
weight of evidence
Study period:
2017-05-30 to 2017-08-07
Reliability:
2 (reliable with restrictions)
Rationale for reliability incl. deficiencies:
guideline study with acceptable restrictions
Reason / purpose:
reference to same study
Qualifier:
according to
Guideline:
other: OECD Guideline 104 (Vapour Pressure Curve)
Version / remarks:
2006
Deviations:
no
GLP compliance:
yes (incl. certificate)
Type of method:
other: capillary tube method
Key result
Melting / freezing pt.:
>= 56 - <= 76 °C
Atm. press.:
1 013 hPa
Remarks on result:
other: In a preliminary test the melting behaviour of the test item was determined by Capillary method, Decomposition and Sublimation were not investigated

The melting point of the test item was checked by an optical method. The test item changed its colour at approx. 56 °C and started to melt. At a temperature of approx. 76 °C the test item was completely molten.

Conclusions:
In a study according to OECD test guideline 104 (2006) a preliminary test was performed in order to determine the melting behaviour of Compimide 183. Melting of the substance was optically determined. The substance began to melt at 56°C and was completely molten at 76°C, thus the melting point of the test item is considered to be 76°C.
Endpoint:
melting point/freezing point
Remarks:
results were obtained from a study according to OECD 113
Type of information:
experimental study
Adequacy of study:
weight of evidence
Study period:
2017-06-06 to 2017-08-08
Reliability:
2 (reliable with restrictions)
Rationale for reliability incl. deficiencies:
guideline study with acceptable restrictions
Reason / purpose:
reference to same study
Qualifier:
according to
Guideline:
other: OECD Guideline 113 (Screening Test for Thermal Stability and Stability in Air)
Version / remarks:
1981
Deviations:
no
GLP compliance:
yes (incl. certificate)
Type of method:
differential scanning calorimetry
Key result
Melting / freezing pt.:
>= 50 - <= 60 °C
Atm. press.:
1 013 hPa
Decomposition:
yes
Decomp. temp.:
>= 150 - <= 300 °C
Sublimation:
no
Remarks on result:
other: Detection of an endothermic peak at 50 -60°C followed by an exothermic peak at 227.36 and 225.98°C, respectively

In the DSC-measurements the test item Compimide 183 showed a first exothermic effect in the temperature range of 150 - 300 °C with an averaged energy release of -210 J/g. A second exothermic effect occurred in the temperature range of 400 to >500 °C with an averaged energy release of >-370 J/g. During both measurements a small, but sharp endothermic peak was observed at a temperature of approximately 50 to 60°C.

Conclusions:
In a study conducted according to OECD test guideline 113 (1981) which was performed in order to measure the thermal stability, a small but sharp endothermic peak was also detected during the DSC measurement. Thus, the substance is considered to melt at approximately 50 to 60°C.

Description of key information

- no melting point detectable: study according to OECD test guideline 102, GLP

- endothermic peak during DSC at 50 -60°C: study according to OECD test guideline 113, GLP

- preliminary test during detection of vapour pressure, Melting point 56 -76°C: study according to OECD test guideline 104, GLP

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:
76 °C

Additional information

In a study performed according to OECD Test Guideline 102 in order to determine the melting point of Compimide 183 a differential scanning calorimetry (DSC) was performed. In a DSC a sample of the test item and a reference material are subjected to the same controlled temperature program. The difference in the temperatures of the test item and the reference material is recorded and applying a calibration function converted to a heat flow signal. When the sample undergoes a transition involving a change in enthalpy (endothermic on melting or boiling), that change is indicated by a departure from the base line of the heat flow record. The course of the thermogravimetric curve between 88 and 451°C suggests decomposition of the test item at approx. 160°C and  no sharp endothermic peak indicating a melting point could be observed, thus, Compimide 183 was considered to decompose but exhibits no melting or boiling point. However, the DSC curve showed a somewhat flunctuating course at a temperature of approximately 80°C and a glass transition was reported at 35°C.

In a study conducted according to OECD test guideline 113 (1981) which was performed in order to measure the thermal stability, a small but sharp endothermic peak was also detected during the DSC measurement. Thus, the substance is considered to melt at approximately 50 to 60°C.

In a study according to OECD test guideline 104 (2006) a preliminary test was performed in order to determine the melting behaviour of Compimide 183. Melting of the substance was optically determined. The substance began to melt at 56°C and was completely molten at 76°C, thus the melting point of the test item is considered to be 76°C.

The melting point of Compimide was determined with two different methods. During the DSC measurements no defined endothermic peak was observed although the results revealed a reaction at lower temperatures. The results of the optically determination of the melting point substantiate the assumption that Compimide has a low melting point. The melting point of the test item is considered to be 76°C based on the optical detection in a preliminary test conducted during the determination of vapour pressure.