4-chloromethyl-4''-ethyl-2'-fluoro-[1,1':4',1''-terphenyl]

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:

06.-26.07.2017

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Qualifier:

according to guideline

Guideline:

EU Method A.1 (Melting / Freezing Temperature)

GLP compliance:

no

Type of method:

differential scanning calorimetry

Key result

Melting / freezing pt.:

>= 102 - <= 140 °C

Atm. press.:

1 013 hPa

Decomposition:

no

Melting point / melting range: DSC measurement

Two DSC measurements with a heating rate of 10 K/min showed an endothermal effect (melting) in the temperature range of 100 - 120 °C. Another two-phase endothermal effect was observed in the temperature range of 130 - 150 °C. 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. The first measurement showed an exothermal effect starting 175 °C (this effect could have been caused by a reaction with the material of the crucible.

The results of the DSC measurements are summarized in Table 1.

Table 1: 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
36358	14.34	25	500	100 - 120 130 - 150	104.05 multistage	Aluminium with a hole	Mass loss: 37 %
36361	11.17	25	170	100 - 115 130 - 150	102.62 multistage	Aluminium with a hole	Test item was an orange melt  No mass loss

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

Melting point / melting range: 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 Table 2.

Table 2: Results of the capillary method

No.	Set point/°C	Heating rate/ K/min	Endpoint/ °C	Remarks
1	80	10	160	Approx. 135 °C: test item started to melt Approx. 142 °C: test item appeared melted and clear

 

 

Conclusions:

The melting point of the test substance is in the range 102 -140 °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 three endothermal effects. The first was observed with an onset temperature of 102 - 105 °C in the DSC-measurement (optical observation: no effect was observed). The second endothermal effect consisted of two phases. During the first phase (starting at approximately 130 °C) the test item started to melt. During the second phase (starting at approximately 140 °C) the test item melted completely to a clear liquid.

Description of key information

A study was conducted according to OECD test guideline 102, Regulation (EC) No 440/2008 method A.1. The melting point 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 three endothermal effects. The first was observed with an onset temperature of 102 - 105 °C in the DSC-measurement (optical observation: no effect was observed). The second endothermal effect consisted of two phases. During the first phase (starting at approximately 130 °C) the test item started to melt. During the second phase (starting at approximately 140 °C) the test item melted completely to a clear liquid.