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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:
02.11.2018-27.02.2019
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Qualifier:
according to guideline
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
Version / remarks:
EC No. 440/2008
Deviations:
no
Qualifier:
according to guideline
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Deviations:
no
GLP compliance:
no
Type of method:
differential scanning calorimetry
Key result
Melting / freezing pt.:
> 30 - < 260 °C
Atm. press.:
ca. 1 013.25 hPa
Decomposition:
no
Remarks on result:
other: many transitions and completely molten at 260°C

DSC Measurement

Two DSC measurements with a heating rate of 10 K/min showed an ambiguous course of the baseline with no clear melting point (onset) in the whole temperature range of the DSC measurement (25 - 500 °C).

Ident No. Test item / mg Starting temperature / °C Final test temperature / °C Temperature range (endothermal) / °C Crucible Observation after the measurement
38320 12.24 25 500 no sharp endothermal effects Aluminium with a hole Test item was an orange to brown solidified melt, mass loss: aprox. 1%
38324 11.9 25 500 no sharp endothermal effects Aluminium with a hole Test item was an orange to brown solidified melt, mass loss: aprox. 1%

An additional measurement with the capillary method was performed in order to clarify the results of the DSC measurements.

Capillary tube in a metal block

Further measurements with the capillary method were performed to clarify the results of the DSC measurements. The filling height of the test item in the capillaries/tubes was approximately 5 mm. Measurement 1 and 2 were performed in a melting capillary using a high heating rate of 1 K/min. Measurement 3 was performed in a boiling point tube with a boiling point capillary using a heating rate of 10 K/min.

No. Set Point / °C Heating Rate / K/min End point / °C Remarks
1 150 1 210 150 °C: test item is still a slightly yellow solid but appeared partially molten
Approx.178 °C: test item appeared glassy (slightly turbid)
Approx. 203 °C: test item appeared glassy and got more turbid
2 140 1 210 140 °C: test item is still a slightly yellow solid but appeared partially molten
Approx.175 °C: test item appeared glassy (slightly turbid)
Approx. 192 °C: test item appeared glassy and got more turbid
3 30 10 400 30 °C to 40 °C: slightly yellow solid test item started to melt very partially, boiling point capillary on the top of the sample
Approx.176 °C: test item shrinks and appeared glassy (slightly turbid).Approx. 195 °C: test item appeared glassy and got more turbid.
Approx. 210 °C: boiling point capillary starts to immerge into the test item.
Approx. 222 °C: boiling point capillary is completely immerged into the test item, test item is a turbid liquid
Approx. 260 °C: test item appeared clear and colourless
up to 400 °C: test item appeared clear and slightly yellow

Between 30 °C to 40 °C the test item started to melt partially. At approx. 175 °C to 178 °C the item got glassy with solid particles. During further heating the glassy

test item became liquid and the solid particles were completely molten at approx. 260 °C. Under consideration of the results of the DSC measurements and the capillary method it was assumed that the test item is a mainly amorphic solid with crystalline parts and therefore behaves glassy during heating up.

Conclusions:
The DSC measurements (25 - 500 °C) showed no clear melting point (onset). The test item had a broad melting range of approx. 30 - 260 °C.
Executive summary:

A study was conducted according to OECD test guideline 102, Regulation (EC) No 440/2008 method A.1. The melting point / melting range was determined by differential scanning calorimetry (DSC). The test item and the reference are heated up from the starting temperature to the final temperature at a constant heating rate in a defined atmosphere (nitrogen). Open crucibles are used as containers for the test item and as empty reference crucible. The quantity of heat absorbed or released is measured and recorded. The DSC measurements (25 - 500 °C) showed no clear melting point (onset). The test item had a broad melting range of approx. 30 - 260 °C.

Description of key information

The test item had a broad melting range of approx. 30 - 260 °C.

Key value for chemical safety assessment

Additional information

A study was conducted according to OECD test guideline 102, Regulation (EC) No 440/2008 method A.1.The melting point / melting range was determined by differential scanning calorimetry (DSC). The test item and the reference are heated up from the starting temperature to the final temperature at a constant heating rate in a defined atmosphere (nitrogen). Open crucibles are used as containers for the test item and as empty reference crucible. The quantity of heat absorbed or released is measured and recorded. The DSC measurements (25 - 500 °C) showed no clear melting point (onset). The test item had a broad melting range of approx. 30 - 260 °C.