N-[4-(2',7'-ditert-butyl-9,9'-spirobi[fluorene]-2-yl)phenyl]-9,9-dimethyl-N-(2-phenylphenyl)fluoren-2-amine

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:

25.07.-22-08.2019

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Qualifier:

according to guideline

Guideline:

EU Method A.1 (Melting / Freezing Temperature)

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.:

> 500 °C

Atm. press.:

ca. 1 013.25 hPa

Decomposition:

no

Remarks on result:

not determinable

Remarks:

no melting point up to 500 °C.

DSC measurement

Three DSC measurements with a heating rate of 10K/min in aluminium crucibles with a hole showed an endothermal effect (melting) in the temperature range of 150 - 180°C with onset temperatures of 160.31°C, 160.17°C and 160.17°C, respectively. The onset temperature (see Table 1) was derived from the intersection of the tangent line with the highest slope of the endothermal peak with the baseline.

 

Melting point (DSC measurements)

Ident No.	Test item/ mg	Starting temperature / °C	Final test temperature / °C	Temperature range (melting) /°C	Onset / °C	Crucible	Observations after the measurement
38755	12.41	25	500	155 - 175	160.31	Aluminium with a hole	The test item was an orange melt, no mass loss.
38757	7.42	25	550	150 - 180	160.17	Aluminium with a hole	Test item was a black residue, mass loss 28%.
38759	7.89	25	200	155 - 175	160.17	Aluminium with a hole	The test item was a white melt.

 

An additional measurement with the capillary method was performed in order to clarify the melting behavior.

capillary tube in a metal block

A measurement with the capillary method was performed to clarify the results of the DSC measurements. Since this measurement was performed only as a verifying screening a high heating rate of 10 K/min was chosen and therefore the absolute temperature values derived with the capillary method are not as accurate as the DSC results. The filling height of the test item was approximately 5 mm. The results are summarized in the table below.

Table 2: Results of the capillary method

No.	Set point/°C	Heating rate/ K/min	Endpoint/ °C	Remarks
1	100	10	200	Approx. 100 "C: the light-yellow solid test item appeared unchanged, but small drops were observed at the surface of the capillary Approx. 190.5 °C: the test item started to appear glassy Approx. 200 °C: no further change (test item is still a solid and not melted)

The capillary method measurement showed that the test item got glassy at around 190 °C but did not melt up to 200 °C.

Under consideration of the results from the DSC measurements (small endothermal peak with an onset at 160 °C) and the capillary method (test item got glassy) it was concluded that the test item did

not melt up to 500 °C. The test item had no melting range/point up to 500 °C.

Conclusions:

The test item had no melting range/point up to 500 °C.

Executive summary:

A study was conducted according to OECD test guideline 102, Regulation (EC) No 440/2008 method A.1. The melting range was determined by differential scanning calorimetry. 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. A measurement with the capillary method was performed to clarify the results of the DSC measurements.

The test item showed an endothermal effect at a temperature range of 150 -180 °C in the DSC measurement (optical observation: test item started to melt). The capillary method measurement showed that the test item got glassy at around 190 °C but did not melt up to 200 °C. Under consideration of the results from the DSC measurements (small endothermal peak with an onset at 160 °C) and the capillary method (test item got glassy) it was concluded that the test item did not melt up to 500 °C. The test item had no melting range/point up to 500 °C.

Description of key information

The test item had no melting point/range up to 500 °C.

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) supported by the capillary method showed no clear melting point (onset) up to 500 °C.