lithium bis(fluorosulfonyl)imide

Melting point / freezing point

Administrative data

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

The study was conducted between 18 October 2012 and 21 January 2013.

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2013

Report date:

2013

Materials and methods

Test guideline

Test guideline 1

Qualifier:

according to guideline

Guideline:

OECD Guideline 102 (Melting point / Melting Range)

Test guideline 2

Qualifier:

according to guideline

Guideline:

EU Method A.1 (Melting / Freezing Temperature)

Test guideline 3

Qualifier:

according to guideline

Guideline:

EPA OPPTS 830.7200 (Melting Point / Melting Range)

GLP compliance:

yes (incl. QA statement)

Type of method:

differential scanning calorimetry

Test material

Test material information

Constituent 1

Reference substance name:

lithium(1+) bis(fluorosulfonyl)azanide

EC Number:

924-516-9

Cas Number:

171611-11-3

Molecular formula:

(FSO2)2NLi

IUPAC Name:

lithium(1+) bis(fluorosulfonyl)azanide

Specific details on test material used for the study:

The specific details of the sample used for the test were as follows:
Description: White powder
Batch No.: 11031840006
Purity/Composition: 99%
Test substance storage: At room temperature in the dark desiccated
Stability under storage conditions: Stable
Expiry date: 20 June 2013
Purity/composition correction factor required: No
Hygroscopic: Yes, store in well-sealed container

Results and discussion

Melting / freezing point

Decomposition:

yes

Decomp. temp.:

>= 80 °C

Remarks on result:

other: Unable to determine melting point as substance decomposed upon heating from 80°C.

Any other information on results incl. tables

Preliminary test:

From 325°C upwards the weight of the sample decreased significantly. At 343°C the sample weight had decreased by 25%.

After the experiment, white/grey residue was observed on the lid of the sample container and a beige residue remained in the sample container (original colour: white). The change of the colour indicated reaction and/or decomposition of the test substance.

Main study:

An endothermic peak followed by an exothermic peak was observed between 100°C and 150°C. The effect was most likely obtained due to evaporation of water or melting and reaction and/or decomposition of the test substance. A small second exothermic peak was observed between 175°C and 225°C and a third exothermic was observed starting at 275°C. The latter two effects were due to reaction and/or decomposition of the test substance. After the experiment, a light brown residue was observed on the lid of the sample

container and a brown molten residue remained in the sample container.

To further investigate the effect between 100°C and 150°C three experiments (Experiment II to IV) were performed. Experiment II was stopped after the effect.

In Experiment III a lower heating rate of 5°C/minute was applied. The exothermic effect shifted to lower temperature and started at 80°C. This confirmed that the effect was due to reaction and/or decomposition of the test substance. The endothermic effect shifted to higher temperature, which indicated that melting did not cause the endothermic effect. After

the experiment, a colourless molten residue remained in the sample container.

In Experiment IV a repeated heating cycle was applied. During cooling no effects were observed. With the second heating an exothermic peak followed by an endothermic peak was observed between 70°C and 150°C. It is not known what caused these effects, probably reaction and/or decomposition. After the experiment, a colourless molten residue remained in the sample container.

Applicant's summary and conclusion

Conclusions:

Using DSC, reaction and/or decomposition of Lithium bis(fluorosulfonyl)Imide was observed starting at a temperature of 80°C (353K). Melting and/or boiling of the test substance was not observed. Based on this, the test substance has no melting and/or boiling temperature.

Executive summary:

Using DSC, reaction and/or decomposition of Lithium bis(fluorosulfonyl)imide was observed starting at a temperature of 80°C (353K), therefore no melting temperature was observed. The test was designed in accordance to Method Al Melting/Freezing Temperature of Commission Regulation (EC) No 440/2008 of 30 May 2008, Method 102 of the OECD Guidelines for Testing of Chemicals, 27 July 1995 and United States Environmental Protection Agency (EPA), Product Properties Test Guidelines no. OPPTS 830.7200 of March 1998.