Alkali metal tetrakis (perfluoro-alcoholato)metallate

Boiling point

Link to relevant study record(s)

Reference

Endpoint:

boiling point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

April - May 2020

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Qualifier:

according to guideline

Guideline:

OECD Guideline 103 (Boiling Point)

Version / remarks:

version 27.7.1995

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Type of method:

differential scanning calorimetry

Specific details on test material used for the study:

Designation in Test Facility: 19110701G
Production date: 12. Aug. 2019
Date of Receipt: 07. Nov. 2019
Expiry date: 31. Oct. 2022

Key result

Atm. press.:

1 atm

Decomposition:

yes

Decomp. temp.:

ca. 117.35 °C

Remarks on result:

not determinable

Remarks:

The boiling point could not be determined due to decomposition of the substance starting at 117.35 °C.

Results from Pre-test following Siwoloboff

All observations of the Pre-test following Siwoloboff are presented in the following table:

Table 1: Pre-test following Siwoloboff

Observations	Temperatures in °C
Colorless condensate was visible	Since 120
Condensate at the surface boiled with steam vortex in test tube, the surface was wet and shrivelled	Since 160
steam came out from the test tube, steam vortex was still visible	Since 180
The upper part (the half amount of the test item) was slightly shrivelled	Since 240
Condensate dropped and fizzed, condensate boiled on the wall of the test tube no more liquid on the surface but steam vortex	Since 275
Less condensate and steam	Since 330
No more condensate only a little steam, the test item was slight darker and no more shrivelled	Since 370
Gas burner was turned off	400

 

After cooling down the test item was still solid but getting brownish (beige) and was compacted again, no more shrivelled. The amount of the test item had decreased, and decomposition was considered.

Security Pre-test for the DSC instrument

The crucible was found visually unchanged after reaching a temperature of 450 °C. The weight of the crucible was recorded with 45.04 mg (47.56 mg before experiment).

Calibration of DSC instrument: After calibration with indium and zinc the measurement of indium yielded the following values:

Table 2: Pre-test following Siwoloboff

ExpectedMelting point	Measured Melting point	Expected Energy	Measured Energy	Assessment
156.6 ± 1.0°C	156.62 °C (onset)	28.45 ± 1.0 J/g	28.36 J/g	OK

 

The measurement of indium after calibration met the validity criteria.

 

DSC Measurement of the Test Item: Three determinations were performed and the results are reported in the following table:

Table 3: DSCValues and observations

	Mass test item	Mass crucible (before measurement):	Mass crucible (after measurement):	Observations
First Measurement	2.65mg	47.40mg	45.02 mg	After the test the crucible was visually unchanged The crucible was opened, a few test item was remained as a white solid (slightly shrivelled white powder)
Second Measurement	2.61mg	47.06 mg	44.83 mg	After the test the crucible was visually unchanged
Third Measurement	2.72mg	47.39 mg	45.10 mg	After the test the crucible was visually unchanged.

 

Interpretation of the measurements

Three DSC measurements were performed. In all measurements two endothermic events and one small flat exothermic event were detected.

According to the observations of the pre-test, these events could be an indication of the splitting of a chemical compound. The first endothermic event matches the observation of the pre-test, where condensate with steam was first seen in the test tube. The second endothermic event could correspond to the surface boiling seen in the pre-test. The exothermic event could correspond to the phase where clumping and discoloration were seen. Therefore, no boiling point can be determined under these circumstances.

Validity: Calibration (see above) was valid, but as no boiling point could be determined, no validity needs to be considered.

The determination of boiling point of AM(pfa)4 was determined via DSC (differential scanning calorimetry). Three DSC measurements were performed. In all measurements two endothermic events and one small flat exothermic event were detected. According to the observations of the pre-test, these events could be an indication of the splitting of a chemical compound. No boiling of the test item was observed. Therefore, no boiling point can be determined under these circumstances.

The onset temperature of the first endothermic event, associated with decomposition, resulting as mean from three experiments was found being 117.35 ±0.6 °C, considered as decomposition temperature of the substance.

No observations were made which might cause doubts on the validity of the study out-come. Therefore, the result of the study is considered valid.

Conclusions:

The onset temperature of the first endothermic event, associated with decomposition, was found being 117.35 ±0.6 °C.

Executive summary:

The determination of boiling point of AM(pfa)4 was determined via DSC (differential scanning calorimetry). Three DSC measurements were performed and in all measurements two endothermic events and one small flat exothermic event were detected. According to the observations of the pre-test, these events could be an indication of the splitting of a chemical compound.

The first endothermic event matches the observation of the pre-test, where condensate with steam was first seen in the test tube. The second endothermic event could correspond to the surface boiling seen in the pre-test. The exothermic event could correspond to the phase where clumping and discoloration were seen. Hence, no boiling of the test item was observed. Therefore, no boiling point can be determined under these circumstances.

Description of key information

The determination of boiling point of AM(pfa)4 was determined via DSC (differential scanning calorimetry). Three DSC measurements were performed and in all measurements two endothermic events and one small flat exothermic event were detected. According to the observations of the pre-test, these events could be an indication of the splitting of a chemical compound.

The first endothermic event matches the observation of the pre-test, where condensate with steam was first seen in the test tube. The second endothermic event could correspond to the surface boiling seen in the pre-test. The exothermic event could correspond to the phase where clumping and discoloration were seen. Hence, no boiling of the test item was observed. Therefore, no boiling point can be determined under these circumstances.The onset temperature of the first endothermic event, associated with decomposition, resulting as mean from three experiments was found being 117.35 ±0.6 °C, considered as decomposition temperature of the substance.