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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:
11 January 2018 to 16 February 2018
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:
27 July 1995
Deviations:
no
GLP compliance:
yes (incl. QA statement)
Type of method:
differential scanning calorimetry
Specific details on test material used for the study:
- Appearance: Viscous amber liquid (determined by CharlesRiver Den Bosch)
- Purity/Composition: >85%
- Test item storage: At room temperature

Additional information
- Test Facility test item number: 209080/A
- Purity/Composition correction factor: No correction factor required
- Test item handling: No specific handling conditions required
- Molecular structure: Not indicated
- Molecular formula: C63H116O12
- Molecular weight: 1065.6
Key result
Melting / freezing pt.:
>= -55.4 - <= 4.6 °C
Atm. press.:
ca. 1 013 hPa

Preliminary Test

The TGA curve of the test item is shown in Figure 1. Starting at 350°C, the weight of the sample decreased significantly. At 411°C, the sample weight had decreased by 25%.

After the experiment, an orange molten residue remained in the sample container (original colour: amber). The change of the colour indicated reaction and/or decomposition of the test item.

 

Main Study

The DSC curve obtained with Experiment 1 is shown in Figure 2. During cooling three exothermic peaks were observed (results are archived in the raw data). These exothermic peaks were observed between 0°C and -70°C. These effects were attributed to crystallization of the test item.

During heating three endothermic effects were observed. The first appeared between -80°C and -25°C and had an extrapolated onset temperature of -55.096°C. The effect was most likely obtained due to melting of a part of the test item. The second and the third endothermic peaks were observed between -25°C and 25°C and were not completely resolved. Therefore, an extrapolated onset could not be determined. The peak maximum of the third peak was 4.800°C. The effects were most likely obtained due to melting of parts of the test item. An endothermic effect was starting at 300°C. The endothermic effect was probably obtained due to reaction and/or decomposition of the test item.

After the experiment, a light yellow molten residue remained in the sample container (original colour: amber). The change of the colour indicated reaction and/or decomposition of the test item

Experiment 2 was performed as a duplicate of Experiment 1. Figure 3 shows the DSC curve obtained. Similar results as in Experiment 1 were obtained. The extrapolated onset of the first melting peak was -55.729°C. The peak maximum of the third peak was 4.485°C . After the experiment the residue was unchanged in the sample container. 

The melting temperature was determined as a melting range obtained from the average extrapolated onset of the first melting temperature (-55.4°C) and the average peak maximum of the last melting temperature (4.6°C).

Conclusions:
The melting and boiling temperature of Hetester HCA were determined by DSC.
The melting temperature ofthe test itemwas -55.4°C – 4.6°C (217.7K – 277.8K).
Reaction and/or decomposition of the test itemwas observed during DSC experiment at temperatures of > 300°C (> 573K). Boiling of the test item was not observed below the temperature at which reaction and/or decomposition started. Based on this, the test item has no boiling temperature.
Executive summary:

In this guideline (OECD 102) study, the melting point of the test substance (EC 205-363-0) was found to be -55.4°C – 4.6°C at 1013 hPa.

Description of key information

Study conducted to recognised testing guidelines.

Key value for chemical safety assessment

Additional information

Melting point is -55.4°C – 4.6°C

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