1,2-Bis[2-(1,1,2-trifluoro-2-heptafluoropropyloxy-ethylsulfany)-ethoxycarbonyl]-ethanesulfonate sodium salt

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:

2018-03-28 to 2018-05-30

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

Specific details on test material used for the study:

The sample was tested as received. No further preliminary treatment such as drying or milling was performed. The results given in this report only apply to the tested sample.

Key result

Atm. press.:

1 013.25 hPa

Decomposition:

yes

Decomp. temp.:

>= 200 °C

Melting point / melting range

Two DSC measurements in aluminium crucibles with a hole showed an ambiguous endothermal effect after the melting in the temperature range of 260 - 285 °C.

 

DSC measurements

Test item / mg	Starting temperature / °C	Final test temperature / °C	Temperature range (endo- thermal) / °C	Onset / °C	Crucible	Observations after the measurement
11.07	25	500	260-285	multi- stage	Aluminium with a hole	Test item was discoloured to black, mass loss 94 %
21.18	25	280	260 - 280	multi- stage	Aluminium with a hole	Test item was discoloured to black, mass loss 71 %

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

 

Results of the capillary method

No.	Set point / °C	Heating rate / K/min	End point / °C	Remarks
1	200	10	300	Approx. 200 °C: test item appeared melted Approx. 225 °C: starting formation of bubbles Approx. 235 °C: test item discoloured to orange Approx. 250 °C: test item rose in the capillary and left the observation window
2	30	10	200	Approx. 30 °C. test item appeared unchanged Approx. 79 °C: test item started to melt Approx. 132 °C; test item clear, appeared melted Approx. 200 °C: no further changes, upon inspection the test item was still highly viscous

 

The test item was a waxy solid. According to information from the sponsor it tends to be inhomogeneous with small inclusions of solvent. Under consideration of the results from the DSC measurements, the capillary method and the aforementioned properties it was concluded that the test item exhibited a phase transition around 80 °C (value is subject to a uncertainty of approx. 10 K due to high heating rate). The observed bubbles could have been caused by the release of minor quantities of residual solvent (see also certificate of analysis). As the DSC measurements showed no endothermal effects below 260 °C it had to be assumed that the test item had no melting point.

 

The formation of bubbles above 200 °C might indicate boiling or decomposition or both. Under consideration of the results from the DSC measurements and the capillary method it was concluded that the test item started to decompose under possible boiling above 200 °C.

Conclusions:

The test item showed no distinctive melting. The test item undergoes a phase transition at 80 °C and has not melting point up to the decomposition temperature of 200 °C.

Executive summary:

A study was conducted according to OECD test guideline 102, Regulation (EC) No 440/2008 method A.1 and EPA OCSPP test guideline 830.7200 to determine the melting point of the test item using differential scanning calorimetry. The test item was weighed out into an aluminium crucible under an inert atmosphere (nitrogen). Two tests with about 11 – 21 mg of the test item were performed. As reference crucible, an empty aluminium crucible was used. The substance is a waxy solid at ambient conditions. The crucibles were heated up from room temperature to 500 °C and 280 °C respectively. Two DSC measurements showed an ambiguous endothermal effect after the melting in the temperature range of 260 - 280 °C. An additional measurement with the capillary method was performed in order to clarify the melting range. Since this measurement was performed only as a verifying screening a high heating rate of 10 K/min was chosen. The filling height of the test item was approximately 5 mm. Under consideration of the results from the DSC measurements, the capillary method and the aforementioned properties it was concluded that the test item exhibited a phase transition around 80 °C. The test item showed no distinctive melting. The test item undergoes a phase transition at 80 °C and has not melting point up to the decomposition temperature of 200 °C.

Description of key information

The test item showed no distinctive melting. The test item undergoes a phase transition at 80 °C and has not melting point up to the decomposition temperature of 200 °C (reference 4.2-1).

Additional information

A study was conducted according to OECD test guideline 102, Regulation (EC) No 440/2008 method A.1 and EPA OCSPP test guideline 830.7200 to determine the melting point of the test item using differential scanning calorimetry (reference 4.2-1). The test item was weighed out into an aluminium crucible under an inert atmosphere (nitrogen). Two tests with about 11 – 21 mg of the test item were performed. As reference crucible, an empty aluminium crucible was used. The substance is a waxy solid at ambient conditions. The crucibles were heated up from room temperature to 500 °C and 280 °C respectively. Two DSC measurements showed an ambiguous endothermal effect after the melting in the temperature range of 260 - 280 °C. An additional measurement with the capillary method was performed in order to clarify the melting range. Since this measurement was performed only as a verifying screening a high heating rate of 10 K/min was chosen. The filling height of the test item was approximately 5 mm. Under consideration of the results from the DSC measurements, the capillary method and the aforementioned properties it was concluded that the test item exhibited a phase transition around 80 °C. The test item showed no distinctive melting. The test item undergoes a phase transition at 80 °C and has not melting point up to the decomposition temperature of 200 °C.