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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:
March 05, 2018
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
test procedure in accordance with generally accepted scientific standards and described in sufficient detail
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:
other: OECD Guideline 113 (Screening Test for Thermal Stability and Stability in Air)
Version / remarks:
adopted May 12, 1981
Deviations:
no
GLP compliance:
yes (incl. QA statement)
Type of method:
differential scanning calorimetry
Decomposition:
yes
Decomp. temp.:
257.9 °C

Before the test, the appearance of the substance was orange powder; after the experiments the test item was blackened and its volume increased in the crucible.

Sample weight [mg] Total loss of Mass (%) Peak Onset of effect [°C] Endset of effect [°C] Left Limit [°C] Right Limit [°C] Energy [J/g]
Replicate 1 3.63 46.8 1 125.61 130.57 119.87 133.55 -7.58
(exothermic)
Replicate 2 4.33 44.8 124.48 128.18 121.51 128.23 -5.70
(exothermic)

Mean

125.045 129.375 120.69 130.89 6.64
Replicate 1 3.63 46.8 2 139.14 145.8 133.60 150.16 21.91
(endothermic)
Replicate 2 4.33 44.8 128.24 147.64 128.24 154.03 28.97
(endothermic)

Mean

133.69 146.72 130.92 152.10 25.44
Replicate 1 3.63 46.8 3 209.68 226.96 203.20 236.86 39.96
(endothermic)
Replicate 2 4.33 44.8 219.59 232.99 203.88 238.93 45.44
(endothermic)

Mean

214.635 229.975 203.54 237.90 42.7
Replicate 1 3.63 46.8 4 287.05 333.71 256.19 334.23 -94.51
(exothermic)
Replicate 2 4.33 44.8 297.71 331.45 259.56 332.17 -82.33
(exothermic)

Mean

292.38 332.58 257.88 333.20 -88.42
Replicate 1 3.63 46.8 5 343.5 354.7 334.20 354.63 -146.36
(exothermic)
Replicate 2 4.33 44.8 340.72 351.1 332.25 353.04 -130.67
(exothermic)

Mean

342.11 352.9 333.23 353.84 -138.51

During the heating up phase three endotherm and two exotherm peaks were observed up to 330 °C. During the cooling down phase no thermal effects were observed from 330 to 25 °C.

Sample weight [mg] Measured temperature range (°C) Loss of Mass (%) Observation
4.47 25 - 150 1.8 orange powder
4.29 25 - 230 4.9 dark orange powder
3.92 25 - 260 7.4 dark orange powder
2.63 25 - 330 13.3 black, cohered powder
Conclusions:
The substance decomposes before melt/boil at ca 258 °C.
Executive summary:

The thermal behaviour of the test item was investigated by Differential Scanning Calorimetry method, according to the OECD guidelines 102 and 113. A small amount of test item placed in aluminum cosed crucible and inserted into the furnace of the DSC device. The temperature was increased from 25 to 500 °C with 10 °C/minutes heating rate. The measurement was performed under nitrogen atmosphere. The experiment was performed in duplicate. A supplementary test was run, in order to clarify the substance thermal behavior. A small amount of test item was weighed into a one-way 40 µl aluminum crucible and sealed with closed aluminum lid using a capsule presser. Thus, prepared capsule was inserted into the furnace of the DSC device and heated from 25 to 150, 230, 260 and 330 °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 and the appearance of the test item after the tests, it is concluded the test item started to decompose from 257.9 °C (531.0 K).

Conclusion

The substance decomposes before melt/boil at ca 258 °C.

Description of key information

The substance decomposes before melt/boil at ca 258 °C.

Key value for chemical safety assessment

Additional information

OECD 102/113 - Differential Scanning Calorimetry method