4,4’-Bis[sec-alkyl(C10-C13)phenyl]iodonium tetrakis(pentafluorophenyl)borate

Water solubility

Administrative data

Endpoint:

water solubility

Type of information:

experimental study

Adequacy of study:

key study

Study period:

from 23 January to 13 May 2013

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

other: The result has been considered as reliable without restriction because the test was performed in compliance with OECD and EU guidelines giving scientifically valid results.

Cross-reference

Cross-reference 1

Reason / purpose for cross-reference:

reference to same study

Cross-reference 2

Reason / purpose for cross-reference:

reference to other 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 105 (Water Solubility)

Deviations:

no

Test guideline 2

Qualifier:

according to guideline

Guideline:

EU Method A.6 (Water Solubility)

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Type of method:

flask method

Test material

Test material information

Constituent 1

Reference substance name:

4,4’-Bis[sec-alkyl(C10-C13)phenyl]iodonium tetrakis(pentafluorophenyl)borate

EC Number:

810-260-4

Cas Number:

1115251-57-4

IUPAC Name:

4,4’-Bis[sec-alkyl(C10-C13)phenyl]iodonium tetrakis(pentafluorophenyl)borate

Test material form:

other: viscous liquid

Details on test material:

- Name of test material (as cited in study report): Bis(alkyl(C10-C13)phenyl)iodonium tetrakis(pentafluorophenyl)borate
- Physical state: clear amber liquid
- Batch: 11GP0077
- Date of Receipt: 13 February 2012
- Expiration date of the lot/batch: January 2014
- Storage condition of test material: The test item was stored in a closed vessel at room temperature (20 ± 5 °C) in the dark.
-Stability EtOH: 96 h; H2O, CH3CN, acetone, DMSO: unknown

Results and discussion

Water solubility

Water solubility:

>= 0.02 - <= 0.665 mg/L

Temp.:

20 °C

pH:

>= 5.35 - <= 5.91

Remarks on result:

other: At the plateau the test item concentration, based on cation measurement, lay in the range < 0.02 – 0.355 mg/L and based on anion measurement, in the range of 0.073 – 0.665 mg/L.. Temperature was measured with 19.7 – 20.5 °C.

Details on results:

At the plateau the test item concentration, based on cation measurement, lay in the range < 0.02 – 0.355 mg/L and based on anion measurement, in the range of 0.073 – 0.665 mg/L.. Temperature was measured with 19.7 – 20.5 °C. The wide concentration ranges are probably due to abrasion of the test item and dispersion in the solution. However, no tyndall effect was observed during sampling.

Any other information on results incl. tables

Results:

Measurements for Temperature Dependency of Water Solubility. The data which was acquired for temperature dependency of water solubility is presented in the following table:

Temperature Dependency of Water Solubility

Flask	Temperature in °C	Test Item Conc. (original sample) in mg/L calculated from cation measurement	Test Item Conc. (original sample) in mg/L calculated from anion measurement	Difference to previous sample % Cation	Difference to previous sample % Anion
1	20.3	0.06	0.08	-	-
2	4.0	0.05	0.10	16.7	-25.0

Because the difference between the measured concentrations of the two flasks was below 3 %/°C (1.0 %/°C for cation related measurements and 1.5 %/°C for anion related measurements ), the main study is performed at 20 °C only.

Measurements during Equilibration The data which was acquired during equilibration time (flask 13 A-C) is presented in the following table:

Day	Temperature in °C	Flask	Test Item Conc. in mg/L (calculated from cation measurement)	Test Item Conc. in mg/L (calculated from anion measurement)	Difference to previous sample % Mean Flasks A-C Cation	Difference to previous sample % Mean Flasks A-C Anion
1	20.5	13A	< LOQ	< LOQ	n.c	-
2	20.5	13B	< LOQ	< LOQ	n.c	-
3	20.5	13C	< LOQ	< LOQ	n.c	-
8	20.5	13A	< LOQ	0.020	n.c	n.c
9	20.4	13B	< LOQ	0.037	n.c	n.c
10	20.5	13C	< LOQ	0.025	n.c	n.c
11	19.9	13A	< LOQ	0.045	n.c	87
12	19.9	13B	< LOQ	0.064	n.c	87
13	19.7	13C	< LOQ	0.045	n.c	87
18	20.4	13A	< LOQ	0.054	n.c	29
19	20.3	13B	< LOQ	0.086	n.c	29
20	20.3	13C	< LOQ	0.059	n.c	29
25	20.5	13A	< LOQ	0.116	n.c	155
26	20.5	13B	0.060	0.240	n.c	155
27	20.5	13C	0.029	0.150	n.c	155
36	19.8	13A	< LOQ	0.096	-7	-31
37	19.9	13B	0.041	0.172	-7	-31
38	20.2	13C	< LOQ	0.079	-7	-31

* not calculable

After the analysis of the sample of days 36-38 (864 – 912 hours), the plateau was considered as reached. The evaluation of the measurements of flasks 13 A-C shows high differences between cation and anion concentration, probably due to high uncertainty in measurement at low concentration range. The test item concentration, calculated from measurements of the cation, lay in the range <0.02 -0.06 mg/L and, calculated from measurements of the anion, in the range of <0.02 -0.24 mg/L/

Measurements at Plateau

The concentrations of test item cation and anion were determined from the measured values following the equation which is given in chapter 6.9. The following table gives the values which were measured at the plateau.

Flask	Blank	14	15	16	17	18
pH	5.37	5.91	5.88	5.89	5.53	5.35
Temperature in °C	20.1	20.0	20.4	20.5	19.9	19.7
Nominal concentration in mg/L	0	52	100	202	503	1007
Test item concentration in mg/L (cation based measurement)	<LOQ	<LOQ	0.355	<LOQ	0.154	0.035
Test item concentration in mg/L (anion based measurement)	<LOQ	0.073	0.665	0.068	0.662	0.122

The test item concentration lay in the range <0.02 -0.355 mg/L L(cation based measurement) resp. in the range of 0.073 – 0.665 mg/L (anion based measurement). The wide concentration ranges are probably due to abrasion of the test item and dispersion in the solution. However, no tyndall effect was observed during sampling. Calculation of a mean is not reasonable because of the wide concentration range. The test item does not show concentration dependency of water solubility. The solubility of PI2080 is therefore stated as <0.02 -0.665 mg/L.

Temperature was measured with 19.7 – 20.5 °C.

DISCUSSION

The solubility of PI2080 in water was determined from the measured concentrations of test item cation and anion in the clear test solutions. Centrifugation of the supernatants was performed one time only. Equilibration time can be considered as approx. 600 – 648 hours (25 – 27 days), determined in three flasks. Loading rates were prepared with range 50-1007 mg/L. At the plateau the test < 0.02 – 0.355 mg/L resp., based on anion measurement, in the range of 0.073 – 0.665 mg/L. The wide concentration ranges are probably due to abrasion and dispersion of test item particles in the aqueous solution. Even though no Tyndall effect was visible in the solutions, formation of small amounts of dispersed particles leading to erroneous results cannot be excluded. Calculation of mean is not reasonable because of the wide concentration range. The test item does not show concentration dependency of water solubility. The solubility of PI2080 is therefore stated as < 0.02 – 0.665 mg/L.

Applicant's summary and conclusion

Conclusions:

Interpretation of results (migrated information): slightly soluble (0.1-100 mg/L)
The solubility of PI2080 in water was determined from the measured concentrations of test item cation and anion in the clear test solutions. Centrifugation of the supernatants was performed one time only. Equilibration time can be considered as approx. 600 – 648 hours (25 – 27 days), determined in three flasks. At the plateau the test item concentration, based on cation measurement, lay in the range < 0.02 – 0.355 mg/L resp., based on anion measurement, in the range of 0.073 – 0.665 mg/L.

Executive summary:

This study was performed according to OECD 105 and EU Method A.6 in order to determine the water solubility of PI2080 .

The quantity of test item necessary to saturate the desired volume of water is estimated from the preliminary test. As the measured solubility may be dependent on the amount of the test item which was added to the flasks, different loading rates were chosen to study the effect of loading rate on the measured water solubility. At least five times the amount which was determined in the preliminary study is used. Measurements are performed in one replicate until equilibrium is reached. Then, all replicates were sampled and analysed.

The solubility of PI2080 in water was determined from the measured concentrations of test item cation and anion, in the clear test solutions.

Temperature dependency was not perceived: As the difference between the measuredconcentrations of two flasks with nominal concentration 2000 mg/L which had been stored at 20.3 °C and at 4.0 °C for about 24 hours, was < 3%/°C, the main study was performed

at 20 °C only.

In the main test, as test item-water mixtures, shaken and centrifuged, did not result in clear solutions, caused by formation of colloidal particles, the main test was performed using slow stirring.

During equilibration time, three flasks with the nominal concentration 50 mg/L were sampled.

The sampling period ranged from 1 – 38 days. Equilibration time can be considered

as approx. 600 – 648 hours (25 – 27 days), determined in three flasks.

At the plateau, the test item concentration, calculated from measurement of the cation, lay in the range < 0.02 mg/L(LOQ) – 0.355 mg/L and, calculated from measurement of the anion, in the range of 0.073 – 0.665 mg/L. The wide concentration ranges are probably due to abrasion of the test item and dispersion in the solution. However, no Tyndall effect was observed during sampling.

The test item does not show concentration dependency of water solubility.

The solubility of PI2080 is stated as

< 0.02 – 0.355 mg/L at 20.0 ± 0.5 °C calculated from cation measurements and 0.073 – 0.665 mg/L at 20.0 ± 0.5 °C calculated from anion measurements.