4-Ethyl-2’-fluoro-4’-bromobiphenyl

Water solubility

Link to relevant study record(s)

Reference

Endpoint:

water solubility

Type of information:

experimental study

Adequacy of study:

key study

Study period:

2019-03-14 to 2019-03-21

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Qualifier:

according to guideline

Guideline:

OECD Guideline 105 (Water Solubility)

Qualifier:

according to guideline

Guideline:

EU Method A.6 (Water Solubility)

Deviations:

no

GLP compliance:

no

Type of method:

flask method

Key result

Water solubility:

83 µg/L

Conc. based on:

test mat.

Incubation duration:

51 h

Temp.:

20 °C

pH:

6

Details on results:

In both columns the concentration of five consecutive fractions was constant within ± 30 %. No increasing or decreasing tendency was observed. The water solubility of the test item was determiend to be 83 µg/L (± 2 µg/L) (mean value of the columns).

Preliminary test

Three preliminary tests were carried out with specified amounts of the test item and 100 mL and 500 mL demineralized water, respectively. After each addition of an amount of water, the mixture was stirred for at least 24 hours, and visually checked for any undissolved particles.

 

Results of the preliminary test

Amount of test item / mg	Total volume of demineralized water / mL	Appearance of mixture
10.4	100	not dissolved
11.5	500	not dissolved
4.2	500	not dissolved

 

The preliminary test showed that the water solubility of the test item was below 10 mg/L. According to the preliminary test the water solubility was determined by the column elution method in the main test.

 

Column elution method

107.5 mg of the test item were dissolved in 100 mL acetone. For charging the columns in each case 25 mL of the test item solution was added to about 3 g of sea sand and the mixtures were shaken. The solvent was then removed under reduced pressure using a rotary evaporator (40 °C, approx. 20 mbar). The dry residues were placed into the columns of the test apparatus, which have afterwards been filled with water (test temperature: 20 °C; water pH at 23 °C: 5.0). After a swelling time of 2 h pumps were started to rinse the test item coated sand with demineralized water. At the end of the study it was confirmed that residual test item remained on the columns. The residual test item was eluted with 50 mL acetone. As blank value demineralized water was tested. No signal was detected in the range of the retention time of the test item. The concentration of the test item was quantified by HPLC.

 

Column 1:

 

Rotation period of the fraction collector 90 min per fraction

Duration of sampling: about 51 h (34 fractions)

 

Column elution method, column 1 (approximately 12.5 mL/h)

Fraction no.	V /mL	pH	water solubility /µg/L
25	20.0	5.9	79
26	20.0	5.9	72
27	20.0	6.0	83
28	20.0	6.0	85
29	20.0	6.0	90

The water solubility was found to be 82 µg/L (± 7 µg/L).

 

Column 2:

Rotation period of the fraction collector 45 min per fraction
Duration of sampling: about 51 h (68 fractions)

 

Column elution method, column 2 (approximately 25.0 mL/h)

Fraction no.	V /mL	pH	water solubility / µg/L
50	15.5	6.0	79
51	15.5	6.0	89
52	15.5	6.0	78
53	15.5	6.0	87
54	15.5	6.0	92

The water solubility was found to be 85 µg/L (± 6 µg/L).

In both columns the concentration of five consecutive fractions was constant within ± 30 %. No increasing or decreasing tendency was observed. The water solubility cs of the test item was 83 µg/L (± 2 µg/L) (mean value of the columns).

Conclusions:

The water solubility of the test item was determined to be 83 µg/L (± 2 µg/L) (mean value of the columns).

Executive summary:

The water solubility of the test item was determined according to OECD 105 and Regulation (EC) No 440/2008 method A.6 using the column elution method with HPLC analysis. 107.5 mg of the test item were dissolved in 100 mL acetone. For charging the columns in each case 25 mL of the test item solution was added to about 3 g of sea sand and the mixtures were shaken. The solvent was then removed under reduced pressure using a rotary evaporator (40 °C, approx. 20 mbar). The dry residues were placed into the columns of the test apparatus, which have afterwards been filled with water (test temperature: 20 °C; water pH at 23 °C: 6.0). After a swelling time of 2 h, pumps were started to rinse the test item coated sand with demineralized water. At the end of the study it was confirmed that residual test item remained on the columns. The concentration of test item was determined by means of HPLC. The pH of each sample was recorded. In both columns the concentration of five consecutive fractions was constant within ± 30 %. No increasing or decreasing tendency was observed. The water solubility of the test item was determined to be 83 µg/L (± 2 µg/L) (mean value of the columns).

Description of key information

The water solubility of the test item was determined to be 83 µg/L (± 2 µg/L) (mean value of the columns).

Key value for chemical safety assessment

Water solubility:

83 µg/L

at the temperature of:

20 °C

Additional information

The water solubility of the test item was determined according to OECD 105 and Regulation (EC) No 440/2008 method A.6 using the column elution method with HPLC analysis (reference 4.8-1). 107.5 mg of the test item were dissolved in 100 mL acetone. For charging the columns in each case 25 mL of the test item solution was added to about 3 g of sea sand and the mixtures were shaken. The solvent was then removed under reduced pressure using a rotary evaporator (40 °C, approx. 20 mbar). The dry residues were placed into the columns of the test apparatus, which have afterwards been filled with water (test temperature: 20 °C; water pH at 23 °C: 6.0). After a swelling time of 2 h, pumps were started to rinse the test item coated sand with demineralized water. At the end of the study it was confirmed that residual test item remained on the columns. The concentration of test item was determined by means of HPLC. The pH of each sample was recorded. In both columns the concentration of five consecutive fractions was constant within ± 30 %. No increasing or decreasing tendency was observed. The water solubility of the test item was determined to be 83 µg/L (± 2 µg/L) (mean value of the columns).