4-(trans-4-Propylcyclohexyl)-1-bromobenzene

Water solubility

Link to relevant study record(s)

Reference

Endpoint:

water solubility

Type of information:

experimental study

Adequacy of study:

key study

Study period:

27.04. - 06.10.06

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Qualifier:

according to guideline

Guideline:

EU Method A.6 (Water Solubility)

Version / remarks:

92/69/EWG

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Type of method:

column elution method

Key result

Water solubility:

0.051 mg/L

Temp.:

20 °C

pH:

> 7.19 - < 7.22

The concentration of the test item in 5 collected fractions was determined by means of HPLC. Therefore, the carrier material was filled into a micro column and was left 2h for swelling.

The circular pump with a flow rate of 25mL/h was started and after 141 h a sample was removed, and the pump was started again. In hourly intervals further samples were taken.

The concentrations were quantified by comparing integrated peak areas with a calibration (external standard method with the test item). The solutions were determined by HPLC.

A second run was done at a flow rate of 12.5 mL/h and with an elution time of 141 h.

Time in h       Sample       Appearance       pH       concentration

Flowrate 25 mL/h

8:45       11       Clear       7.20       0.05

9:45       12       Clear       7.20       0.05

10:45       13       Clear       7.21       0.04

11:45       14       Clear       7.19       0.04

12:45       15       Clear       7.21       0.04

Flowrate 12.5 mL/h

9:30       11       Clear       7.22       0.07

10:30       12       Clear       7.22       0.06

11:30       13       Clear       7.20       0.05

12:30       14       Clear       7.21       0.06

13:30       15       Clear       7.22       0.05

The test material was extracted with acetonitrile from the column, diluted t 100 mL and quantified by HPLC. At flowrates of 25 mL/h and 12.5 mL/h amounts of 12.86 mg and 11.46 mg respectively were detected. The test item was sufficiently adsorbed by the column.

The water solubility was calculated as mean of the both experiments at different flow rates and a solubility of 0.051 mg/L at 20 °C was determined

Conclusions:

The test item has a water solubility of 0.051 mg/L at 20 °C.

Executive summary:

The water solubility was determined according to 92/69/EWG A.6 using the column elution method with HPLC analysis. 2.0018 g of the test item were dissolved in 100 mL methylene dichloride. For charging column 1 (flow rate of approx. 12.5 ml/h) and column 2 (flow rate of approx. 25.0 mL/h) in each case 25 mL of the test item solution was added to about 10 g of silica. The solvent was then removed under reduced pressure using a rotary evaporator (40 °C, 20 mbar) and dried in the vacuum oven at 40 °C for 72 h.700 mg of the loaded silica were added to a micro column filled with 5 mL water and left 2h for swelling. 25 mL water were added, 15 ml water were removed and returned to circulation. The column was filled with 85 mL of water and the circular pump with a flow rate of 25mL/h was started. After 141 h a sample was removed, and the pump was started again. In hourly intervals further samples were taken. The concentrations were quantified by comparing integrated peak areas with a calibration (external standard method with the test item). The solutions were determined by HPLC. The water solubility was calculated as mean of the both experiments at different flow rates and a solubility of 0.051 mg/L at 20 °C was determined

Key value for chemical safety assessment

Water solubility:

0.051 mg/L

at the temperature of:

20 °C

Additional information

The water solubility was determined according to 92/69/EWG A.6 using the column elution method with HPLC analysis. 2.0018 g of the test item were dissolved in 100 mL methylene dichloride. For charging column 1 (flow rate of approx. 12.5 ml/h) and column 2 (flow rate of approx. 25.0 mL/h) in each case 25 mL of the test item solution was added to about 10 g of silica. The solvent was then removed under reduced pressure using a rotary evaporator (40 °C, 20 mbar) and dried in the vacuum oven at 40 °C for 72 h.700 mg of the loaded silica were added to a micro column filled with 5 mL water and left 2h for swelling. 25 mL water were added, 15 ml water were removed and returned to circulation. The column was filled with 85 mL of water and the circular pump with a flow rate of 25mL/h was started. After 141 h a sample was removed, and the pump was started again. In hourly intervals further samples were taken. The concentrations were quantified by comparing integrated peak areas with a calibration (external standard method with the test item). The solutions were determined by HPLC. The water solubility was calculated as mean of the both experiments at different flow rates and a solubility of 0.051 mg/L at 20 °C was determined