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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:
07 March 2018 to 28 March 2018
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Qualifier:
according to
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Deviations:
no
Qualifier:
according to
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
Deviations:
no
Qualifier:
according to
Guideline:
EPA OPPTS 830.7200 (Melting Point / Melting Range)
Deviations:
no
GLP compliance:
yes
Type of method:
differential scanning calorimetry
Melting / freezing pt.:
>= -16.2 - <= 9.1 °C
Remarks on result:
other: glass transition observed at -55.0 °C (218.2K)

PRELIMINARY TEST

- The TGA curve of the test item is shown in Figure 1 (attached).

- Starting at 250°C, the weight of the sample decreased significantly.

- At 309°C, the sample weight had decreased by 25%.

- After the experiment, a colourless residue remained in the sample container (original colour: colourless).

 

MAIN STUDY

- The DSC curve obtained with Experiment 1 is shown inFigure 2(attached). 

- During cooling,an exothermic peak between -25 °C and -10 °C was found (results are archived in the raw data). The effect was obtained due to crystallization of the test item. 

- A glass transition was observed between -70 °C and -40 °C. During heating, a glass transition was observed between -75 °C and -50 °C. 

- The inflection point of the glass transition was -54.595 °C. Exothermic and endothermic peaks were observed between -50°C and 25 °C directly followed by a broad endothermic effect between 25°C and 100°C. 

- The peak maximum of the endothermic peaks were -16.099 °C (first peak), -7.500 °C (second peak) and 9.328 °C (third peak). 

- The exothermic effects were due to crystallisation of the test item.

- The endothermic effects were due to melting of the test item. 

- The broad endothermic effect was due to evaporation of volatile components, based on the weight loss observed during the preliminary test. An endothermic peak was observed starting at 200°C. This endothermic effect was due to reaction and/or decomposition of the test item.

- Experiment 2 was performed to determine duplicate glass transition temperature and duplicate melting temperatures. Figure 3 (attached) shows the DSC curve obtained. The inflection point of the glass transition was -55.349 °C. The peak maximum of the endothermic peaks were -16.277 °C (first peak), -7.693 °C (second peak) and 8.923 °C (third peak). After the experiment, the sample appeared to have been unchanged, i.e. no decomposition and/or evaporation were observed. 

- The glass transition temperature was determined as the mean glass transition temperature of Experiment 1 (-54.595 °C) and Experiment 2 (-55.349 °C).

- The test item is a mixture. Three endothermic melting peaks were observed. Therefore, a melting range was given instead of a melting temperature. The melting range was determined with the melting temperatures obtained with Experiment 1 (-16.099 °C, -7.500 °C and 9.328 °C) and Experiment 2 (-16.277 °C, -7.693 °C and 8.923 °C).

Conclusions:
The melting range of the test item was -16.2 to 9.1 °C (257.0 to 282.3K). A glass transition ofthe test item was observed at -55.0°C (218.2K).
Executive summary:

GUIDELINE

The investigation was conducted in accordance with OECD Guideline 102 Melting Point/Melting Range (July 27, 1995), EC Guideline A.1 Melting/Freezing Temperature (March 04, 2016) and EPAProduct Properties Test Guideline OPPTS 830.7200: Melting Point/Melting Range (March 1998). The melting temperature of the test item was determined by Differential Scanning Calorimetry (DSC).

 

RESULTS

The melting range of the test item was -16.2 to 9.1 °C (257.0 to 282.3K). A glass transition ofthe test item was observed at -55.0°C (218.2K).

Description of key information

The melting range of the test item was -16.2 to 9.1 °C (257.0 to 282.3K). A glass transition of the test item was observed at -55.0°C (218.2K) (OECD 102. EU Method A.1 and OPPTS 830.7200).

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:
-16.2 °C

Additional information

GUIDELINE

The investigation was conducted in accordance with OECD Guideline 102 Melting Point/Melting Range (July 27, 1995), EC Guideline A.1 Melting/Freezing Temperature (March 04, 2016) and EPAProduct Properties Test Guideline OPPTS 830.7200: Melting Point/Melting Range (March 1998). The melting temperature of the test item was determined by Differential Scanning Calorimetry (DSC).

 

RESULTS

The melting range of the test item was -16.2 to 9.1 °C (257.0 to 282.3K). A glass transition of the test item was observed at -55.0 °C (218.2K).