5-Brom-2-[(3,4,5-trifluorphenoxy)-difluormethyl]-1,3-difluorbenzene

Water solubility

Link to relevant study record(s)

Reference

Endpoint:

water solubility

Type of information:

experimental study

Adequacy of study:

key study

Study period:

18.10. - 26.10.06

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Qualifier:

according to guideline

Guideline:

OECD Guideline 105 (Water Solubility)

GLP compliance:

yes (incl. QA statement)

Type of method:

column elution method

Key result

Water solubility:

< 0.01 mg/L

Conc. based on:

test mat.

Temp.:

20 °C

pH:

> 6.5 - < 6.9

Preliminary test

Amounts of the test item and water were stirred at room temperature until the mixture appeared dissolved or the water solubility could be estimated to be below 10 mg/l..

 

Table 1: Appearance of the test mixtures

Amount of test item /mg	Total volume of demineralized water / mL	Appearance of mixture
82.3	0.1	undissolved
	0.5	undissolved
	1.0	undissolved
	2.0	undissolved
	10.0	undissolved
10.9	100	undissolved
11.2	500	undissolved
9.73	1000	undissolved

 

The preliminary test showed that the water solubility of the test item is below 9.73 mg/l (without correction of the purity). According to the preliminary test the water solubility was determined by the column elution method in the main test.

 

Column elution method

Column 1:

Rotation period of the fraction accumulator:         90 min per fraction

Average fraction volume:                                          16.1 ml

Flow rate:                                                                      between 10.7 ml/h and 11.0 ml/h

Duration of sampling:                                               about 69 h (46 fractions)

 

Column 2:

Rotation period of the fraction accumulator:         45 min per fraction

Average fraction volume:                                          16.3 ml

Flow rate:                                                                      between 21.3 ml/h and 22.0 ml/h

Duration of sampling:                                               about 68 h (91 fractions)

Column 3 (blank):

Rotation period of the fraction accumulator:         45 min per fraction

Average fraction volume:                                          16.3 ml

Flow rate:                                                                      between 21.3 ml/h and 22.0 ml/h

Duration of sampling:                                               about 41 h (55 fractions)

Table 1: column elution method, column 1

Fraction no	V / mL	pH	Water solubility in µg/L
16	16.5	6.5	25.2
23	16.0	6.7	35.5
24	16.0	6.6	39.9
25	16.0	6.8	19.0
26	16.0	6.7	20.5
27	16.0	6.7	20.5
28	16.0	6.5	24.7
29	16.0	6.8	20.8
40	16.0	6.8	< 8.07
41	16.0	6.9	< 8.07
42	16.0	6.8	< 8.07
43	16.0	6.8	< 8.07
44	16.0	6.8	< 8.07

 

According to the guideline the run can be stopped if the concentrations of five fractions do not differ more than +/- 30 % without any raising or descending tendency. The content of test item in the fractions 40 to 44 is below the detection limit.

 

Table 2: column elution method, column 2

Fraction no	V / mL	pH	Water solubility in µg/l
32	16.5	6.5	43.3
51	16.5	6.6	54.3
52	16.5	6.7	59.7
53	16.5	6.7	33.4
54	16.5	6.7	24.0
55	16.5	6.5	19.2
79	16.0	6.9	11.6
80	16.0	6.8	10.6
81	16.0	6.8	9.08
82	16.0	6.7	< 8.07
83	16.0	6.7	< 8.07
84	16.0	6.6	< 8.07
85	16.0	6.7	< 8.07
86	16.0	6.7	< 8.07

 

According to the guideline the run can be stopped if the concentrations of five fractions do not differ more than +/- 30 % without any raising or descending tendency. The content of test item in the fractions 82 to 86 is below the detection limit.

 

Table 3: Column elution method: Column 3 (blank)

Fraction no.	V in ml	pH	water solubility in µg/l
28	16.5	6.8	< 8.07
29	16.5	6.7	< 8.07
30	16.5	6.7	< 8.07
31	16.5	6.9	< 8.07
32	16.5	6.8	< 8.07

 

According to the guideline, the data of the fractions 1 to 5 were not taken into account for the following evaluation. The values for the water solubility were calculated from fractions 40 to 44 for column 1, from the fractions 82 to 86 for column 2, from the fractions 28 to 32 for column 3.

Result column 1:

Evaluation of fraction 40 to 44:

The water solubility was found to be: < 8.07 µg/l (without correction of the purity)

Result column 2:

Evaluation of fraction 82 to 86:

The water solubility was found to be: < 8.07 µg/l (without correction of the purity)

Result column 3:

Evaluation of fraction 28 to 32:

The blank concentration was found to be: < 8.07 µg/l.

Coating check:

Table 4: Coating check

	Amount of test item used for coating /mg	Measured concentration of  test item in eluate /mg/L	Amount of test item  eluated /mg
Column 1	22.2	276.0 / 274.0	13.8
Column 2	22.2	318.7 / 317.8	15.9

 

The coating check was successful.

 

Conclusions:

The water solubility cs of the test item at a temperature of 20°C was determined according to the column elution method. It was found to be below the quantification limit: cs < 0.01 mg/l.

Executive summary:

The water solubility was determined according to OECD 105 using the column elution method. The preliminary test showed that the water solubility of the test item is < 10 mg/L. The column elution method showed a solubility: cs < 8.07 µg/L or < 0.01 mg/l.

Description of key information

The water solubility was determined according to OECD 105 using the column elution method. The preliminary test showed that the water solubility of the test item is < 10 mg/L. The column elution method showed a solubility below the quantification limit: cs < 8.07 µg/L or < 0.01 mg/l.