Reaction mass of rel-(2R,3aR,6R,7aR)-2,6-dimethyl-3a-(propan-2-yl)octahydro-1-benzofuran and rel-(2R,3aR,6S,7aR)-2,6-dimethyl-3a-(propan-2-yl)octahydro-1-benzofuran and rel-(2R,3aS,6S,7aS)-2,6-dimethyl-3a-(propan-2-yl)octahydro-1-benzofuran

Water solubility

Link to relevant study record(s)

Reference

Endpoint:

water solubility

Type of information:

experimental study

Adequacy of study:

key study

Study period:

The study was conducted between 22 May 2014 and 23 August 2014.

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Remarks:

The study is considered to be a reliability 1 as it has been conducted according to OECD Test Guideline 105 using a slow stir adaptation of the flask method and in compliance with GLP.

Qualifier:

according to guideline

Guideline:

OECD Guideline 105 (Water Solubility)

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Type of method:

flask method

Water solubility:

0.049 g/L

Temp.:

20 °C

pH:

>= 6.6 - <= 6.9

Details on results:

Preliminary Test
The preliminary estimate of water solubility was 4.90E-02 g/L at 20.0 °C.

Main Test
No significant response was obtained within the retention time window of the test item in any sample matrix blanks or standard matrix blanks on analysis.

Equilibrium Preliminary Sampling
Equilibrium evident from approximately 121 hours

Vessel 1
Mean concentration: 4.93E-02 g/L at 20.0 ± 0.5 ºC
Range: 4.87E-02 to 5.02E-02 g/L
Standard deviation: 6.32E-04

Vessel 2
Mean concentration: 4.94E-02 g/L at 20.0 ± 0.5 ºC
Range: 4.89E-02 to 4.98E-02 g/L
Standard deviation: 4.05E-04

Vessel 3
Mean concentration: 4.92E-02 g/L at 20.0 ± 0.5 ºC
Range: 4.72E-02 to 5.06E-02 g/L
Standard deviation: 1.58E-03

Overall water solubility
Overall mean water solubility: 4.93E-02 g/L at 20.0 ± 0.5 ºC
Overall standard deviation: 9.18E-04
Relative standard deviation: 1.86%

Compositional information provided by the Sponsor indicated the presence of a number of isomers of the test item (2,6-dimethyl-3a-(propan-2-yl)octahydro-1-benzofuran), which in total represent the reported purity for this substance. Using this information, the calculation of the test item water solubility was calculated based on the total peak area of all peaks obtained on chromatographic analysis which were attributed to these isomers of the test item. On comparison of the relative peak/isomer responses for the test item standard and sample solutions, there was no evidence of significant selective solubility/extractivity, with all test item peaks/isomers being detected, at a similar ratio, on analysis of the water solubility sample solutions.
In the absence of any evidence of selective solubility/extractivity, it was considered unnecessary to evaluate the influence of the initial nominal loading rate on the composition of the dissolved test item fraction.

The mean total peak areas relating to the standard and sample solutions are shown in the following table:

Solution	Mean Total Peak Area
Standard solution, 208 mg/L	1.6756 x 10^7
Standard solution, 213 mg/L	1.7387 x 10^7
Preliminary assessment, sample 1	1.5996 x 10^7
Standard solution, 206 mg/L	1.6614 x 10^7
Standard solution, 202 mg/L	1.6095 x 10^7
Preliminary assessment, sample 2	1.5954 x 10^7
Standard solution, 211 mg/L	1.6966 x 10^7
Standard solution, 208 mg/L	1.6718 x 10^7
Preliminary assessment, sample 3	1.6570 x 10^7

Solution	Mean Total Peak Area
Standard solution, 211 mg/L	1.6997 x 10^7
Standard solution, 208 mg/L	1.6714 x 10^7
Definite test, vessel 1, sample 1	1.5897 x 10^7
Definite test, vessel 2, sample 1	1.6032 x 10^7
Definite test, vessel 3, sample 1	1.5655 x 10^7
Standard solution, 220 mg/L	1.7853 x 10^7
Standard solution, 211 mg/L	1.7225 x 10^7
Definite test, vessel 1, sample 2	1.5972 x 10^7
Definite test, vessel 2, sample 2	1.5999 x 10^7
Definite test, vessel 3, sample 2	1.5367 x 10^7
Standard solution, 236 mg/L	1.9357 x 10^7
Standard solution, 217 mg/L	1.7632 x 10^7
Definite test, vessel 1, sample 3	1.5923 x 10^7
Definite test, vessel 2, sample 3	1.5991 x 10^7
Definite test, vessel 3, sample 3	1.6417 x 10^7
Definite test, vessel 1, sample 4	1.6407 x 10^7
Definite test, vessel 2, sample 4	1.6231 x 10^7
Definite test, vessel 3, sample 4	1.6552 x 10^7

The concentration (g/L) of test item in the sample solutions is shown in the following tables:

Equilibrium Preliminary Sampling

Sample Number	Stirring / Equilibration Time (hours)	Concentration (g/L)	Solution pH
1	121	4.94 x 10^-2	7.7
2	142	4.98 x 10^-2	6.7
3	165	5.15 x 10^-2	6.7

Vessel 1

Sample Number	Stirring / Equilibration Time (hours)	Concentration (g/L)	Solution pH
1	172	4.94 x 10^-2	6.7
2	191	4.91 x 10^-2	6.7
3	216	4.87 x 10^-2	6.9
4	223	5.02 x 10^-2	6.6

Vessel 2

Sample Number	Stirring / Equilibration Time (hours)	Concentration (g/L)	Solution pH
1	172	4.98x 10^-2	6.7
2	191	4.91x 10^-2	6.7
3	216	4.89x 10^-2	6.9
4	223	4.97x 10^-2	6.7

Vessel 3

Sample Number	Stirring / Equilibration Time (hours)	Concentration (g/L)	Solution pH
1	172	4.86x 10^-2	6.7
2	191	4.72x 10^-2	6.6
3	216	5.02x 10^-2	6.9
4	223	5.06x 10^-2	6.6

The overall water solubility results are summarized in the following table:

Vessel	1	2	3
Mean Water Solubility (g/L at 20.0 ± 0.5 ºC)	4.93 x 10^-2	4.94 x 10^-2	4.92 x 10^-2
Standard Deviation	6.32 x 10^-4	4.05 x 10^-4	1.58 x 10^-3

Validation

The linearity of the detector response with respect to concentration was assessed over the nominal concentration range of 25 to 400 mg/L. This was satisfactory with a first order correlation coefficient of 0.9995 being obtained.

 

Recovery of analysis of the sample procedure was assessed and proved adequate for the test. Recovery data is shown in the following table:

Nominal Concentration (mg/L)	Mean Recovery (%)	Number of Replicates (n)	Standard Deviation
50	92.8	5	0.585
10	91.1	5	3.50

Concentrations have not been corrected for recovery of analysis.

Conclusions:

Interpretation of results (migrated information): slightly soluble (0.1-100 mg/L)
The water solubility of the test item was determined to be 4.93E-02 g/L of solution at 20.0 ± 0.5 °C, using a slow stir adaptation of the standard test method. On comparison of the relative peak/isomer responses for the test item standard and sample solutions, there was no evidence of significant selective solubility/extractivity, with all test item peaks/isomers being detected, at a similar ratio, on analysis of the water solubility sample solutions.

Executive summary:

The water solubility of the test substance, IFF 215 (Floraine), was determined to be 4.93E-02 g/L of solution at 20.0 ± 0.5 °C according to OECD Test Guideline 105 using a slow stir adaptation of the flask method. The test substance was therefore considered to be slightly soluble.

Description of key information

The water solubility of the test substance, IFF 215 (Floraine), was determined to be 4.93E-02 g/L of solution at 20.0 ± 0.5 °C according to OECD Test Guideline 105 using a slow stir adaptation of the flask method. The test substance was therefore considered to be slightly soluble.

Key value for chemical safety assessment

Water solubility:

0.049 g/L

at the temperature of:

20 °C