2,3-difluoro-1-propoxy-4-[4-(trans-4-propylcyclohexyl)-1-cyclohexen-1-yl]-benzene

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:

04.-07.07.2017

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.:

>= 52 - <= 163 °C

Atm. press.:

1 013 hPa

Decomposition:

no

Two DSC measurements with a heating rate of 10 K/min showed four endothermal effects (melting) in the temperature range of 50 - 60 °C, 60 - 75 °C, 120 - 140 °C and 155 - 175 °C. The onset temperatures were 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 (endo- thermal) / °C	Onset (melting) / °C	Crucible	Observations after the measurement
36351	7.34	25	500	50-60 60-75 120-140 155-175	52.5 64.2 130.0 162.5	Aluminium with a hole	-
36355	7.64	25	500	50-60 60-75 125-140 155-170	52.2 64.0 130.0 163.2	Aluminium with a hole

 

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

 

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.

Results of the capillary method

No.	Set point / °C	Heating rate / K/min	End point / °C	Remarks
1	25	10	200	Approx. 65 °C: test item started to melt Approx. 68 °C: test item baked together Approx. 131 °C: test item nearly clear slightly cloudy Approx. 164 °C: test item totally molten, no further change observed up to 200 °C

 

The test item showed four endothermal effects. The first was observed with an onset temperature of 52 °C in the DSC-measurement (optical observation: no effect was observed). At the second endothermal effect with an onset temperature of 64 °C (DSC-measurement) the optical observation showed the test item started to melt. At the third endothermal effect at 130 °C onset temperature (DSC-measurement) the test item was slightly cloudy. At the fourth endothermal effect at 163 °C onset temperature (DSC measurement) the test item was observed to be completely molten by optical inspection. Thus, it was concluded that the test item has a melting range from 52 to 163 °C.

Conclusions:

The melting point of the test item was determined to be in the range 52 -163°C.

Executive summary:

A study was conducted according to OECD test guideline 102 and Regulation (EC) No 440/2008 method A.1 to determine the melting point of the test item using 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 were used as containers for the test item and as empty reference crucible. The quantity of heat absorbed or released was measured and recorded. 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 test item showed four endothermal effects. The first was observed with an onset temperature of 52 °C in the DSC-measurement (optical observation: no effect was observed). At the second endothermal effect with an onset temperature of 64 °C (DSC-measurement) the optical observation showed the test item started to melt. At the third endothermal effect at 130 °C onset temperature (DSC-measurement) the test item was slightly cloudy. At the fourth endothermal effect at 163 °C onset temperature (DSC measurement) the test item was observed to be completely molten by optical inspection. Thus, it was concluded that the test item melts in the range from 52 to 163 °C.

Description of key information

The melting point of the test item was determined to be in the range 52 -163°C (reference 4.2 -1).

Additional information

A study was conducted according to OECD test guideline 102 and Regulation (EC) No 440/2008 method A.1 to determine the melting point of the test item using 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 were used as containers for the test item and as empty reference crucible. The quantity of heat absorbed or released was measured and recorded. 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 test item showed four endothermal effects. The first was observed with an onset temperature of 52 °C in the DSC-measurement (optical observation: no effect was observed). At the second endothermal effect with an onset temperature of 64 °C (DSC-measurement) the optical observation showed the test item started to melt. At the third endothermal effect at 130 °C onset temperature (DSC-measurement) the test item was slightly cloudy. At the fourth endothermal effect at 163 °C onset temperature (DSC measurement) the test item was observed to be completely molten by optical inspection. Thus, it was concluded that the test item melts in the range from 52 to 163 °C.