lithium bis(fluorosulfonyl)imide

Particle size distribution (Granulometry)

Administrative data

Endpoint:

particle size distribution (granulometry)

Type of information:

experimental study

Adequacy of study:

key study

Study period:

The study was conducted between 25 October 2012 and 23 November 2012.

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2012

Report date:

2012

Materials and methods

Test guideline

Test guideline 1

Qualifier:

according to guideline

Guideline:

ISO 13320 (Particle size analysis - Laser diffraction methods)

Test guideline 2

Qualifier:

according to guideline

Guideline:

other: CTL SOP No. 417

GLP compliance:

yes (incl. QA statement)

Type of method:

microscopic examination

Remarks:

Followed by Laser Diffraction Particle Size Analyser

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 on the test material used in this study were as follows:
Description: White powder
Batch number: 11031840006
Purity: 99 %
Test substance storage: At room temperature in the dark. Sample is hygroscopic, store in well-sealed container
Stability under storage conditions: Stable
Expiry date: 20 June 2013 (allocated by WIL Research Europe B.V., 1 year after receipt of the test substance)
Relative density: 2.32 (supplied by WIL Research Europe B.V.)

Results and discussion

Mass median aerodynamic diameter:

1 538.2 µm

Geometric standard deviation:

0.02

Particle size distribution at different passages

Particle size distribution at different passages 1

No.:

#1

Size:

< 544.762 µm

Distribution:

10 %

Particle size distribution at different passages 2

No.:

#2

Size:

< 1 009.883 µm

Distribution:

50 %

Particle size distribution at different passages 3

No.:

#3

Size:

< 1 579.384 µm

Distribution:

90 %

Any other information on results incl. tables

Full Test Results:

	Run 1	Run 2	Run 3	Run 4	Run 5	**Average
Volume weighted Mean	1008.098	1029.464	1047.632	1057.585	990.982	1026.752
Median (d. 50)	989.878	1009.730	1030.128	1048.722	970.281	1009.883
Mode (µm)	1081.862	1103.013	1123.404	1151.969	1057.683	1106.429
*MMAD	1507.730	1537.970	1569.040	1597.360	1477.880	1538.200
10% of material is <	524.398	553.505	574.208	567.662	509.840	544.762
50% of material is <	989.878	1009.730	1030.128	1048.722	970.281	1009.883
90% of material is <	1563.290	1580.523	1592.782	1606.604	1547.784	1579.384

All results are in μm

* Mass Median Aerodynamic Diameter

**Average result is calculated from the entirety of data captured in each run and is not a

simple arithmetic mean.

0.17 % by volume of sample was seen to be < 10.00 μm.

External ultra-sonication was employed inorder to attempt to disperse the agglomerations. The agglomerations were seen to remain after 20 minutes sonication and some small particle fractures were observed. The final analysis was therefore conducted without sonication.

Standard Deviation results:

Run No.	1	2	3	4	5	STDVP	% STDV
d10	524.398	553.505	574.208	567.662	509.840	24.88	4.56
d50	989.878	1009.730	1030.128	1048.722	970.281	27.88	2.76
d90	1563.290	1580.523	1592.782	1606.604	1547.784	20.84	1.32
d15.78	619.723	642.215	662.800	667.879	603.386	24.70	3.86
*GSD	1.597	1.572	1.554	1.570	1.608	0.02	1.24
MMAD	1507.730	1537.970	1569.040	1597.360	1477.880	42.47	2.76

*GSD = Geometric standard deviation

Coefficient of variation for d50 is less than 3%; d10 and d90 are less than 5%. Thus repeatability of the characteristic particles in the size distribution are within the acceptable limits as per the ISO 13320-1 test standard.

Applicant's summary and conclusion

Conclusions:

Due to the sample being highly hygroscopic, the analysis was conducted using the small volume (wet) module (SVM) with silicone oil as the dispersant. The laser diffraction test conducted to determine the particle size analysis produced the following results (results are an average in µm):

Volume weighted mean: 1026.752
Median (d.50) 1009.883
Mode 1106.429
MMAD (Mass Median Aerodynamic Diameter) 1538.20
10% of material is < 544.762
50% of material is < 1009.883
90% of material is < 1579.384

0.17 % by volume of sample was seen to be < 10.00 μm.

Executive summary:

Due to the sample being highly hygroscopic, the analysis was conducted using the small volume (wet) module (SVM) with silicone oil as the dispersant. The laser diffraction test conducted to determine the particle size analysis produced the following results:

	Average (µm)
Volume weighted mean	1026.752
Median (d.50)	1009.883
Mode	1106.429
MMAD (Mass Median Aerodynamic Diameter)	1538.20
10% of material is <	544.762
50% of material is <	1009.883
90% of material is <	1579.384

0.17 % by volume of sample was seen to be < 10.00 μm.

The test was conducted in accordance with ISO 13320 - Particle size analysis and Laser Diffraction methods, and CTL SOP No. 417.