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Melting point / freezing point

Link to relevant study record(s)

Reference

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

April 23, 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

Specific details on test material used for the study:

The test item was finely ground using a mortar and a pestle.

Decomposition:

yes

Decomp. temp.:

257.8 °C

Before the test, the appearance of the test item was dark blue powder. After the experiments the test item became a black powder in the crucible.

During the heating the test item showed exothermic signal from approx. 257 °C which was assumed to be decomposition of the test item.

	Sample weight [mg]	Total loss of Mass of the Sample [%]	Left Limit [°C]	Right Limit [°C]	Onset of effect [°C]	Endset of effect [°C]	Energy [J/g]
Rep. 1	3.98	31.7	150.82	169.91	151.61	154.34	168.15 (endothermic)
			257.88	430.31	336.13	409.38	-200.96 (exothermic)
Rep. 2	4.75	26.3	168.78	193.27	169.58	172.43	67.98 (endothermic)
			257.8	423.06	335.43	402.9	-213.63 (exothermic)

		Experiment 1	Experiment 2	Mean
Endothermic peak	Onset of effect [°C]	151.61	169.58	160.6
	Endset of effect [°C]	154.34	172.43	163.39
	Energy [J/g]	168.15	67.98	118.07
Exothermic peak	Left Limit [°C]	257.88	257.8	257.84
	Right Limit [°C]	430.31	423.06	426.69
	Energy [J/g]	-200.96	-213.63	-207.3

Conclusions:

Decomposition before melting/boiling at ca 257.8 °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 closed 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.

Before the test, the appearance of the test item was dark blue powder; after the experiments the test item became a black powder in the crucible.

The endotherm and exotherm peaks in the thermograms do not imply phase transition from a solid to liquid state. Using a linear heating rate melting point was not observed from room temperature up to 500 °C.

Based on the results of the DSC curves and the appearance of test item after the tests, it is concluded the test item started to decompose from 257.8 °C (531.0 K).

Conclusion

Decomposition before melting/boiling at ca 257.8 °C

Description of key information

Decomposition before melting/boiling at ca 257.8 °C

Additional information

OECD 102/113 - differential scanning calorimetry