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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:
September from 21st to 22nd, 2017
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Qualifier:
according to guideline
Guideline:
other: OECD guideline 113 (Screening Test for Thermal Stability and Stability in Air)
Version / remarks:
adopted May 12, 1981
Deviations:
no
Qualifier:
according to guideline
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Version / remarks:
adopted July 27, 1995
Deviations:
no
Qualifier:
according to guideline
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
Deviations:
no
Qualifier:
according to guideline
Guideline:
EPA OPPTS 830.7200 (Melting Point / Melting Range)
Deviations:
no
GLP compliance:
yes
Type of method:
differential scanning calorimetry
Specific details on test material used for the study:
The test item was used in its initial form.
Decomposition:
yes
Decomp. temp.:
ca. 109 °C
Remarks on result:
other: endothermic decomposition
Decomposition:
yes
Decomp. temp.:
ca. 180 °C
Remarks on result:
other: exothermic decomposition

Summary of the DSC test of test item

Experiment 1 Experiment 2 Mean
Endotherm peak Onset of effect [°C] 109.20 109.20 109.20
Endset of effect [°C] 117.03 117.68 117.36
Energy [J/g] -2.96 -2.76 -2.86
Exotherm contiguous peak Left limit [°C] 182.40 182.15 182.28
Right limit [°C] 223.64 219.45 221.55
Energy [J/g] 88.17 91.58 89.88

Values of the DSC run in the first experiment

Sample weight [mg] Total loss of mass (%) Onset of effect [°C] Endset of effect [°C] Left limit [°C] Right limit [°C] Energy [J/g]
2.50 63.2 109.20 117.03 106.27 119.88 2.96 (endothermic)
212.39 223.61 182.40 223.64 -88.17 (exothermic)

Values of the DSC run in the second experiment

Sample weight [mg] Total loss of Mass (%) Onset of effect [°C] Endset of effect [°C] Left Limit [°C] Right Limit [°C] Energy [J/g]
2.70 61.9 109.20 117.68 106.27 119.74 2.76 (endothermic)
207.72 219.45 182.15 219.45 -91.58 (exothermic)

SECOND EXPERIMENT

During the heating up phase endothermic signals were observed in the temperature range of approx. 108 – 170 °C. During the cooling down phase no thermal effects were observed from 205 to 25 °C.

Values of the DSC run in the Supplementary Test 1

Sample weight [mg] Loss of Mass (%) Temperature range [°C] Observation
2.75 1.1 25 – 120 light, reddish brown powder

Values of the DSC run in the Supplementary Test 2

Sample weight [mg] Loss of Mass (%) Temperature range [°C] Observation
2.29 5.2 25 – 140 reddish brown powder

Values of the DSC run in the Supplementary Test 3

Sample weight [mg] Loss of Mass (%) Temperature range [°C] Observation
2.83 6.4 25 – 180 dark grey, clumped powder

Values of the DSC run in the Supplementary Test 4

Sample weight [mg] Loss of Mass (%) Temperature range [°C] Observation
2.81 20.6 25 – 205 black melt with shiny green surface; bubbles were visible in the melt

APPEARANCE OF THE SAMPLE IN THE MAIN TEST

Before the test, the substance appeared as an orange powder. After the experiments the test item melted and blackened in the crucible.

Conclusions:
Endothermic decomposition starts at 109.20 °C; exothermic decomposition starts before melting at ca. 180 °C.
Executive summary:

The thermal behaviour of the substance was investigated using the differential scanning calorimetry method, in accordance with the OECD guidelines 102 and 113.

In the first experiment, the prepared capsule was inserted into the furnace of the DSC device and heated from 25 to 500 °C with 10 °C/minutes heating rate. The measurement was performed under nitrogen atmosphere. Before and after the test, the weight and the appearance of the sample were determined. This experiment was performed in duplicate.

A supplementary test was run, in order to clarify the thermal behavior of the substance. The prepared capsule was inserted into the furnace of the DSC device and heated from 25 to 120 °C, 140 °C, 180 °C and 205 °C with 10 °C/minutes heating rate, than cooled down to 25 °C. Before and after the test, the weight and the appearance of the sample were determined.

Based on the results of the DSC curves, exothermic decomposition occurs between ca. 180 and 220 °C; based on results and appearance of test item after the supplementary tests, it is concluded that an endothermic decomposition starts from ca. 109 °C.

Description of key information

Endothermic decomposition starts at 109.20 °C; exothermic decomposition starts before melting at ca. 180 °C.

Key value for chemical safety assessment

Additional information

OECD 102 and 113 - differential scanning calorimetry method