Reaction mass of (1RS)-1-[(1RS)-3,3-dimethylcyclohexyl]ethyl [(2RS,3RS)-3-ethyloxiran-2-yl]acetate and (1RS)-1-[(1RS)-3,3-dimethylcyclohexyl]ethyl [(2SR,3SR)-3-ethyloxiran-2-yl]acetate and (1RS)-1-[(1SR)-3,3-dimethylcyclohexyl]ethyl [(2RS,3RS)-3-ethyloxiran-2-yl]acetate and (1RS)-1-[(1SR)-3,3-dimethylcyclohexyl]ethyl [(2SR,3SR)-3-ethyloxiran-2-yl]acetate

Water solubility

Link to relevant study record(s)

Reference

Endpoint:

water solubility

Type of information:

experimental study

Adequacy of study:

key study

Study period:

5-05-2014 to 13-05-2014

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

other: Guideline study performed under GLP. All relevant validity criteria were met.

Qualifier:

according to guideline

Guideline:

OECD Guideline 105 (Water Solubility)

Deviations:

no

Qualifier:

according to guideline

Guideline:

EU Method A.6 (Water Solubility)

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Remarks:

inspected: June 2013; signature: November 2013

Type of method:

flask method

Water solubility:

13.2 mg/L

Conc. based on:

test mat.

Incubation duration:

96 h

Temp.:

20 °C

pH:

8

Remarks on result:

other: mean of 24, 48 and 72 h in duplicate measurements tested after 96 hours incubation; (n =6)

Preliminary test:

A non-GLP preliminary test has been performed to determine the application dose used in the definitive study. For this purpose, 3 replicates of a water: test item mixture at an application dose of approx. 1 g/L were mixed overnight (approx. 24 h) and the aqueous phase was centrifuged (10 m in at 10000 x g and 20 °C) analysed via GC-MS.Due to the application procedure, instead of the fivefold 100 µL of the test item were transferred directly as layer onto 100 mL double distilled water. The determined solubility was in the range of 7 mg/L.

 

Definitive test:

The solubility of the test item in double distilled water was determined employing the flask method at 20 ± 0.5 °C with preincubation at 30 ± 0.5 °C. The water solubility was respectively at pH 8.0:

 

Table 1. Water solubility (96 h incubation – measured after 96 h at 20 ± 0.5 °C)

Preincubation time / hours	Replicate	Measured concentration #1 / mg/L	Mean / mg/L
24	1	10.3
	2	22.0	16.2
48	1	13.5
	2	15.5	14.5
72	1	12.0
	2	11.8	11.9
Mean (48 – 72 h)			13.2
Deviation / % #2			22.0
CV / % #3			13.4

#1 Mean value of triplicate samples, single injected, dilution factor 500

#2 Calculated

#3 Coefficient of variation after 48- 72 h preincubation

 

Temperatures were kept constant within ± 0.5 °C. The determined solubilities of the two test vessels difference by more than 15 %, however this was deemed acceptable see below. The analytical method (SPME-GC-MS, external standard) for the determination of the test item was validated and tested with satisfactory results in regard to linearity, accuracy, precision and specificity. The water solubility was determined 24 and 96 h after reduction to test temperature (20°C). The results obtained for the first measurement (24 h after reduction to test temperature) were slightly outside the calibration range and therefore only used for comparison. A plateau phase was reached. The second set of samples (96 h after reduction to test temperature) gave more scattering results, but as they are comparable to the first measurement they were used to calculate the water solubility. The concentrations, measured for the two longest pre-incubation times (48 and 72 h) of the sampling after 96 h of incubation, differed for 22%. This deviation was considered to be negligible, as the results obtained from an additional sampling (results slightly out of calibration range, therefore not used for evaluation) after 24 h of incubation showed comparable and less differing (7%) results, proving that plateau phase was reached.

Conclusions:

Interpretation of results: slightly soluble (0.1-100 mg/L)
The test item water solubility was determined to be 13.2 mg/L at pH 8.0 and 20.0 °C.

Executive summary:

The water solubility of the substance was determined according to OECD Method 105 and EU Method A.6 in accordance with GLP. Determinations with preincubation at 30 ± 0.5 °C and stirring rate of 300 rpm for 24, 48 and 72 hours respectively. After preincubation the temperature was deuced to the test temperature of 20 ± 0.5 °C for 24 h and secondary for 96 h with stirring at approx. 100 rpm. The analytical method (SPME-GC-MS, external standard) for the determination of the test item was validated and tested with satisfactory results in regard to linearity, accuracy, precision and specificity. Temperatures were kept constant within ± 0.5 °C. The determined solubilities of the two test vessels difference by more than 15 %, however this was deemed acceptable see below. The analytical method (SPME-GC-MS, external standard) for the determination of the test item was validated and tested with satisfactory results in regard to linearity, accuracy, precision and specificity. The water solubility was determined 24 and 96 h after reduction to test temperature (20°C). The results obtained for the first measurement (24 h after reduction to test temperature) were slightly outside the calibration range and therefore only used for comparison. A plateau phase was reached. The second set of samples (96 h after reduction to test temperature) gave more scattering results, but as they are comparable to the first measurement they were used to calculate the water solubility. The concentrations, measured for the two longest pre-incubation times (48 and 72 h) of the sampling after 96 h of incubation, differed for 22%. This deviation was considered to be negligible, as the results obtained from an additional sampling (results slightly out of calibration range, therefore not used for evaluation) after 24 h of incubation showed comparable and less differing (7%) results, proving that plateau phase was reached. The water solubility of each isomer contributing to the purity of the test item was determined to be 10.6 mg/L. The water solubility was also determined for the test item as a whole. Under the conditions of this study, the mean water solubility of the substance was determined to be 13.2 mg/L at 20 ± 0.5 °and pH 8.0.

Description of key information

Water Solubility: 13.2 mg/L at pH 8.0 and 20 °C, flask method - OECD TG 105, 2016

Key value for chemical safety assessment

Water solubility:

13.2 mg/L

at the temperature of:

20 °C

Additional information

Key study : OECD TG 105, 2016 : The water solubility of the substance was determined according to OECD Method 105 and EU Method A.6 in accordance with GLP. Determinations with preincubation at 30 ± 0.5 °C and stirring rate of 300 rpm for 24, 48 and 72 hours respectively. After preincubation the temperature was deuced to the test temperature of 20 ± 0.5 °C for 24 h and secondary for 96 h with stirring at approx. 100 rpm. The analytical method (SPME-GC-MS, external standard) for the determination of the test item was validated and tested with satisfactory results in regard to linearity, accuracy, precision and specificity. Temperatures were kept constant within ± 0.5 °C. The determined solubilities of the two test vessels difference by more than 15 %, however this was deemed acceptable see below. The analytical method (SPME-GC-MS, external standard) for the determination of the test item was validated and tested with satisfactory results in regard to linearity, accuracy, precision and specificity. The water solubility was determined 24 and 96 h after reduction to test temperature (20°C). The results obtained for the first measurement (24 h after reduction to test temperature) were slightly outside the calibration range and therefore only used for comparison. A plateau phase was reached. The second set of samples (96 h after reduction to test temperature) gave more scattering results, but as they are comparable to the first measurement they were used to calculate the water solubility. The concentrations, measured for the two longest pre-incubation times (48 and 72 h) of the sampling after 96 h of incubation, differed for 22%. This deviation was considered to be negligible, as the results obtained from an additional sampling (results slightly out of calibration range, therefore not used for evaluation) after 24 h of incubation showed comparable and less differing (7%) results, proving that plateau phase was reached. The water solubility of each isomer contributing to the purity of the test item was determined to be 10.6 mg/L. The water solubility was also determined for the test item as a whole. Under the conditions of this study, the mean water solubility of the substance was determined to be 13.2 mg/L at 20 ± 0.5 °and pH 8.0.