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Physical & Chemical properties

Boiling point

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Reference
Endpoint:
boiling point
Type of information:
experimental study
Adequacy of study:
key study
Study period:
From 30-September-2016 to 22-December-2016
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Remarks:
GLP compliant
Qualifier:
according to
Guideline:
EU Method A.2 (Boiling Temperature)
Deviations:
no
Qualifier:
according to
Guideline:
OECD Guideline 103 (Boiling Point)
Deviations:
no
GLP compliance:
yes (incl. certificate)
Remarks:
Inspection dates: 13 - 15 October 2015 / Date of the certificate: 13 January 2016
Type of method:
method according to Siwoloboff
Remarks:
Four runs were completed with the DSC method. As variable and inconsistent results were obtained, a visual test (Siwoloboff method) was performed.
Key result
Boiling pt.:
121.2 °C
Atm. press.:
102.5 kPa
Decomposition:
no
Remarks on result:
other: Value corrected due to baromtric pressure
Remarks:
Mean value from two runs

Results of the Differential Scanning Calorimetry

Test A

The test was conducted in an open aluminium crucible. The sample was observed to undergo two endothermic events, the first commenced at 124.92°C which had an endothermic heat of boiling of 51.15 J.g-1 and the second commenced at 339.06°C (9.84 J.g-1 ) On completion of the test the crucible was observed to be empty.

Test B

The test was conducted in an open aluminium crucible. The sample was observed to undergo an endothermic event from 115.89°C (99.46 J.g-1 ). On completion of the test the crucible was observed to be empty.

Test C

The test was conducted in an open aluminium crucible. The sample was observed to undergo an endothermic event from 151.23°C (77.23 J.g-1 ). On completion of the test brown residue remained in the crucible.

Test D

The test was conducted in an open aluminium crucible. The sample was observed to undergo an endothermic event from 68.71°C (118.28 J.g-1 ). On completion of the test the crucible was observed to be empty.

Results of the Siwoloboff method

 Run Number  Mass of sample used (g)  Boiling temperature (°C)
 1  0.4  121.4
 2  0.3  122.1
 Mean boiling temperature (°C) 121.8    
       Result: 121.8 °C (Corrected due to barometric pressure)

The sample produced a regular stream of bubbles from 107°C.

Conclusions:
The boiling point of Fluorosulfonic Adduct is 121.2 °C at 102.5 kPa.
Executive summary:

The determination of the boiling point of Fluorosulfonic Adduct was performed under GLP compliance in accordance with the OECD Guideline No. 103 and the EU Method A.2.

In a first time, four runs with the Differential Scanning Calorimetry method was performed. A sample of Fluorosulfonic Adduct was charged to an open aluminium DSC crucible which was then placed in the furnace. The sample was then ramped from 25°C to 500°C at 4 K/min. An empty cell, similarly prepared, was used as a reference pan. The sample and reference pans were then placed into a furnace which was heated to 25°C. Once the pans had equilibrated with the furnace, the cells were heated at a constant rate (of up to 20 K.min-1 ) up to 500°C. Microcomputer data logging was used to monitor the power output of the sample and the temperature in the oven.

Results obtained through the 4 runs were variable and inconsistent, therefore the test site decided to perform a visual test (Siwoloboff method).

In a second time, the Siwoloboff method was used to determine the boiling point of the Fluorosulfonic adduct. The sample was charged to a sample tube & a boiling capillary. The sample was then heated at 3°C/min, which was reduced to 1°C/min at about 10°C below the expected boiling point. When the boiling temperature was approached, bubbles began to emerge rapidly from the capillary. The boiling point was defined as the temperature at which on momentary cooling, the bubbles stopped and fluid started rising in the capillary.

The boiling point of Fluorosulfonic Adduct was 121.2 °C at 102.5 kPa.

Description of key information

The boiling point of Fluorosulfonic Adduct was 121.2 °C at 102.5 kPa.

Key value for chemical safety assessment

Boiling point at 101 325 Pa:
121.2 °C

Additional information

The determination of the boiling point of Fluorosulfonic Adduct was performed under GLP compliance in accordance with the OECD Guideline No. 103 and the EU Method A.2.

Two methods were used for determination of the boiling point for Fluorosulfonic adduct: the Differential Scanning Calorimetry (DSC) method and the Siwoloboff method.

The Differential Scanning Calorimetry (DSC) method was used first. As the DSC method provided variable and inconsistent results the boiling points was determined by a visual test according to the Siwoloboff method.

The boiling point of Fluorosulfonic Adduct was determined to be 121.2 °C at 102.5 kPa.