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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:
18 Oct 2017 to 01 Nov 2017
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
GLP compliance:
yes (incl. certificate)
Type of method:
differential scanning calorimetry
Specific details on test material used for the study:
SOURCE OF TEST MATERIAL
- Source and lot/batch No.of test material: Sponsor and ZMG-197685
- Expiration date of the lot/batch: 09 December 2017
- Purity test date: 28 December 2016
Key result
Melting / freezing pt.:
< -80 °C
Atm. press.:
ca. 1 011 hPa

The TGA curve of the test item is shown inFigure 1. Starting at 130°C, the weight of the sample decreased significantly. At 169°C, the sample weight had decreased by 25%.

After the experiment it was observed that the test item was evaporated from the sample container.

The DSC curve obtained with Experiment 1 is shown inFigure 2. During cooling no effects were observed. During heating anendothermic peak was observed between 125°C and 200°C. The extrapolated onset temperature of the peak was 174.819°C. The endothermic effect was most likely obtained due to boiling of the test item. 

After the experiment it was observed that the test item had evaporated from the sample container.

In order to confirm whetherboiling caused the endothermicpeak, a higher heating rate of 50°C/minute was used in the Experiment 2. Figure 3shows the DSC curve obtained. Theextrapolated onset temperature was 175.465°C. The endothermic peak had not shifted to higher temperatures. It demonstrated that boiling of the test item caused the endothermic effect. After the experiment it was observed that the test item had evaporated from the sample container.

Experiment 3 was performed as a duplicate of Experiment 1. Figure 4shows the DSC curve obtained. Similar results as in Experiment 1 were obtained. The extrapolated onset of theboilingpeak was 174.965°C. After the experiment it was observed that the test item had evaporated from the sample container.

An additional investigation of the melting temperature of the test item was performed placing two subsamples of the test item for 23 hours at -18.6 ± 0.9°C and at -83.8 ± 1.6°C respectively. It was observed after storage that the test item was a liquid (≤ ‑15°C freezer) and a viscous liquid (≤ -80°C freezer). According to this it was concluded that the melting temperature of the test item is ≤ -80°C (< 193K).

Conclusions:
Melting point was not possible to determine during DSC experiment (no effects observed during cooling phase).
The melting temperature of the test item was < -80°C (<193K) applying a storage experiment in the freezer.

Description of key information

Melting point was not possible to determine during DSC experiment (no effects observed during cooling phase).

The melting temperature of the test item was < -80°C (<193K) applying a storage experiment in the freezer.

The atmospheric pressure was 1011 ± 1 hPa.

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:
-80 °C

Additional information