Lithium bis(trifluoromethylsulfonyl)imide

Solubility in organic solvents / fat solubility

Administrative data

Endpoint:

solubility in organic solvents / fat solubility

Type of information:

experimental study

Adequacy of study:

key study

Study period:

From 1992-06-17 to 1993-03-12

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

other: Study performed according to EU Method and according to GLP.

Cross-reference

Reason / purpose for cross-reference:

reference to same study

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

1993

Report date:

1993

Materials and methods

Test guideline

Qualifier:

according to guideline

Guideline:

other: EU Method A.7

Deviations:

yes

Remarks:

EU Method A.7 requires stirring times of 3 and at least 24 hours at 37°C but the laboratory has found these times to be insufficient to reach equilibrium. Therefore times of 24 and 48 hours were used, with a subsequent extended test of 144 hours.

Principles of method if other than guideline:

Fat solubility was determined using a flask-stirring method.

GLP compliance:

yes

Test material

Test material information

Constituent 1

Test material form:

solid: particulate/powder

Details on test material:

Identity: T-4201
Chemical name: Lithium (bis) trifluoromethanesulfonimide
Purity: >99.5%

Results and discussion

Solubility in organic solvents / fat solubility

Medium:

standard fat

Solubility:

42.8 other: g/100 g Standard Fat

Temp.:

37 °C

Test substance stable:

not determined

Details on results:

Calibration data were: yielding slopes, intercepts and correlation coefficients of 9324.5, 23289 and 0.99598 (24, 48-hour analysis) and 9336.7, -4319.3 and 0.99728 (144-hour analysis), showing the detector response to be linear over the concentration range used.

With the 24 and 48-hour analysis, one blank solution chromatogram contained an integrated peak (area = 64398) at the retention volume of the test substance, one contained a small unintegrated peak, and two no peaks. Due to the variable value of these peaks, no correction was made. However, with the 144-hour analysis, the two blank chromatograms contained peaks of a consistent size (areas of 9702, 19391) and the areas of the test and recovery solutions have been corrected by the mean area (14547) before regression analysis.

Procedural recovery data is given in Table 1 (see below "Any other information on results incl.tables"), with recoveries ranging from 96.4 - 110.5%. No correction has been made to the analytical data for these recoveries.

Analytical data are shown in Table 2 (see below "Any other information on results incl.tables"). The results increase with increasing time stirred at 37°C. After 144 hours, the results obtained for the 30°C and 50°C pre-equilibration temperatures agree well, and the mean of these values, 42.8 g/100 g fat, will be quoted as the fat solubility.

Any other information on results incl. tables

Table 1: Recovery data

Analysis	Integrated peak area	Integrated peak area corrected for mean blank area (144-hour only)	Mass of fat analysed (g)	Recovery stock concentration		Recovery (%)
				Analysed (µg/mL)	Nominal (µg/mL)
24 and 48 hours	540945	540945	2.52	13879	12557	110.5
	540462	540462	2.48	13866	12557	110.4
144-hour	438861	424314	2.50	11477	11901	96.4
	461575	447028	2.50	12085	11901	101.5

Table 2: Analytical data

Test conditions		Integrated peak area	Integrated peak area corrected for mean blank area (144-hour only)	Mass of fat analysed (g)	Fat solubility
Hours at 37°C	Temperature stirred at for 1 hour (°C)				g/100 g fat solution (S^1)	g/100 g of fat (S)	Mean result each test g/100 g fat
24	30	322524	322524	2.49	12.888	14.795	11.051
24	30	325167	325167	2.51	12.898	14.808
24	50	157009	157009	2.52	5.6907	6.0341
24	50	210187	210187	2.54	7.8912	8.5673
48	30	521939	521939	2.54	21.054	26.669	29.357
48	30	609392	609392	2.54	24.746	32.883
48	50	559872	559872	2.50	23.018	29.900
48	50	534906	534906	2.51	21.860	27.975
144	30	731876	717329	2.50	30.917	44.753	42.798
144	30	683270	668723	2.52	28.606	40.068
144	50	745577	731030	2.58	30.527	43.941
144	50	705555	691008	2.50	29.789	42.428

Applicant's summary and conclusion

Conclusions:

The fat solubility of bis trifluoromethanesulfonimide lithium was: 42.8 g/100 g Standard Fat at 37°C.

Executive summary:

The determination of the fat solubility of bis trifluoromethanesulfonimide lithium was performed using a flask-stirring method according to EU Method A.7, under GLP conditions. The result was: 42.8 g/100 g Standard Fat at 37°C.