3-Butoxy-7-ethoxy-4,6-difluoro-dibenzothiophene

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:

2016-12-02 to 2016-12-05

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Qualifier:

according to guideline

Guideline:

OECD Guideline 102 (Melting point / Melting Range)

Deviations:

no

Qualifier:

according to guideline

Guideline:

EU Method A.1 (Melting / Freezing Temperature)

Deviations:

no

GLP compliance:

no

Type of method:

differential scanning calorimetry

Key result

Melting / freezing pt.:

80 °C

Atm. press.:

1 013.25 hPa

Decomposition:

no

Sublimation:

no

Melting point / melting range: Differential scanning calorimetry

 

Two DSC measurements with a heating rate of 10 K/min showed a first endothermal effect in the temperature range of 70 - 80 °C and a second endothermal effect in the temperature range of 80 - 90 °C.

 

Melting point (DSC measurements)

Test item / mg	Starting temperature / °C	Final test temperature / °C	Temperature range (melting) / °C	Onset / °C	Crucible	Observations after the measurement
13.67	25	500	70-80 80-90	71.30 79.93	Aluminium with a hole	-
11.54	25	150	70-80 80-90	71.50 80.15	Aluminium with a hole	Test item was a solidified melt

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.

 

Approx. 30 °C: start of measurement, test item was unchanged

Approx. 79 °C: test item started to melt

Approx. 83 °C: test item was fully melted

Approx. 100 °C: no further change

Conclusions:

The melting point was determined to be 80.0 °C at 1013.25 hPa.

Executive summary:

A study was conducted according to OECD TG 102 and Regulation (EC) No 440/2008 method A.1 to determine the melting point of the test item using differential scanning calorimetry and capillary. The test item was weighed into an aluminium crucible under an inert atmosphere (nitrogen). Three tests with about 11 - 13 mg of the test item were performed. As reference crucible, an empty aluminium crucible was used. One DSC measurement with a heating rate of 10 K/min up to the final temperature of 500 °C showed two endothermal effect (melting) in the temperature range of 70 - 90 °C. One additional DSC measurement with a heating rate of 10 K/min up to the final temperature of 150 °C showed two endothermal effect (melting) in the temperature range of 70 -90 °C. A measurement with the capillary method was performed to clarify the results of the DSC measurements. Based on the observations it was concluded that the second enothermal effect with an onset temperature of 80 °C was related to the melting of the test item. Thus, it was concluded that the test item has a melting point of 80.0 °C.

Description of key information

The melting point was determined to be 80.0 °C at 1013.25 hPa.

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:

80 °C

Additional information

A study was conducted according to OECD TG 102 and Regulation (EC) No 440/2008 method A.1 to determine the melting point of the test item using differential scanning calorimetry and capillary (reference 4.2 -1). The test item was weighed into an aluminium crucible under an inert atmosphere (nitrogen). Three tests with about 11 - 13 mg of the test item were performed. As reference crucible, an empty aluminium crucible was used. One DSC measurement with a heating rate of 10 K/min up to the final temperature of 500 °C showed two endothermal effect (melting) in the temperature range of 70 - 90 °C. One additional DSC measurement with a heating rate of 10 K/min up to the final temperature of 150 °C showed two endothermal effect (melting) in the temperature range of 70 -90 °C. A measurement with the capillary method was performed to clarify the results of the DSC measurements. Based on the observations it was concluded that the second enothermal effect with an onset temperature of 80 °C was related to the melting of the test item. Thus, it was concluded that the test item has a melting point of 80.0 °C.