N-[1,1'-Biphenyl]-2-yl-N-[1,1'-biphenyl]-4-yl-9,9'-spirobi[9H-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:

25.08.2016 - 19.12.2016

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:

European Commission Regulation (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.:

> 190 - < 250 °C

Atm. press.:

ca. 1 013.25 hPa

Decomposition:

no

Three DSC measurements in aluminium crucibles with a holeshowed two multisage endothermal effects in the temperature range of 110 - 165°C and 190 - 250 °C with no clear melting point (onset) A third measurement up to 170 °C showed one endothermal effect in the temperature range of 105 - 165 °C. After this effect the test item was partially molten. 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
35809	10.60	25	500	110 - 165 190 - 250	multistage	Aluminium with a hole	Test item was a brown melt Mass loss 0%
35812	10.65	25	250	110 -170 190 - 230	multistage	Aluminium with a hole	Test item was a brown melt Mass loss 0%
35816	12.92	25	170	105 - 165	multistage	Aluminium with a hole	Test item was a brown melt Mass loss 0%

An additional measurement with the capillary method was performed in order to clarify the melting range. The filling height of the test item was approximately 5 mm. The results are summarized in Table 2.

Table 2: Results of the capillary method

No.	Set point/°C	Heating rate/ K/min	Endpoint/ °C	Remarks
1	50	10	250	Approx. 202 °C: test item started to melt Approx. 206 °C: test item molten to silvery white Approx. 218 °C:test item melted and clear with some small bubbles
2	200	1	220	Approx. 215 °C: test item molten to silvery white Approx. 217 °C:test item melted and clear with some small bubbles
3	180	1	200	Approx. 180 °C: test item immediately agglomerated to a shiny white mass

 

The capillary measurements showed that the test item melted within a wide temperature range but did not melt completely up to 250 °C. Under consideration of the results from the DSC measurements and the capillary method it was concluded that the test item melted within a range of 190 - 250 °C. During the melting decomposition started.

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 multistage endothermal effects in the temperature range of 110-165 °C and 190 - 250 °C with no clear melting point. The third measurement up to 170 °C showed one endothermal effect in the temperature range of 105 - 165 °C. An additional measurement with the capillary method was performed in order to clarify the melting range. Under consideration of the results from the DSC measurements and the capillary method, it was concluded that the test item melted within a range of 190 - 250 °C. During the melting decomposition started.

Description of key information

The test item had a melting range of 190 - 250 °C

Additional information

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 multistage endothermal effects in the temperature range of 110-165 °C and 190 - 250 °C with no clear melting point. The third measurement up to 170 °C showed one endothermal effect in the temperature range of 105 - 165 °C. An additional measurement with the capillary method was performed in order to clarify the melting range. Under consideration of the results from the DSC measurements and the capillary method, it was concluded that the test item melted within a range of 190 - 250 °C. During the melting decomposition started.