Reaction mass of 2-(cis-4-methylcyclohexyl)propan-2-ol and 2-(trans-4-methylcyclohexyl)propan-2-ol and cis-1-methyl-4-(propan-2-yl)cyclohexanol and trans-1-methyl-4-(propan-2-yl)cyclohexanol

Water solubility

Link to relevant study record(s)

Reference

Reference 1

Endpoint:

water solubility

Type of information:

experimental study

Adequacy of study:

key study

Study period:

13 June 2013 - 19 June 2013

Reliability:

2 (reliable with restrictions)

Rationale for reliability incl. deficiencies:

other: see "Remark"

Remarks:

The determination of water solubility was performed using the OECD Guideline No 105 (column elution). This study was considered as reliable with restrictions because not enough details on quantification of the substance were reported in the report.

Reason / purpose for cross-reference:

reference to same study

Reason / purpose for cross-reference:

reference to other study

Qualifier:

according to guideline

Guideline:

OECD Guideline 105 (Water Solubility)

Version / remarks:

(27 July 1995)

Deviations:

no

Principles of method if other than guideline:

This method is based on the elution of a test substance with water from a micro-column which is charged with an inert support material (celite), previously coated with an excess of the test substance. The water solubility is given by the mass concentration of the eluate when this has reached a plateau as a function of time. A second experiment is performed at half the flow rate of the first. If the results of the two runs are in agreement, the test is satisfactory. If the measured solubility is higher with the lower flow rate, then the halving of the flow rate must continue until two successive runs give the same solubility.

GLP compliance:

no

Type of method:

column elution method

Key result

Water solubility:

ca. 1 168 mg/L

Temp.:

20 °C

pH:

>= 5 - <= 7

Remarks on result:

other: Measured pH : pH=5.5 at the beginning of the both experiment and pH=7 at the end of the both experiment. The relative difference between the results of the two experiments is 6.16%, less than 30% as required by the OECD 105 - elution column method.

Details on results:

Mean of two solubility values obtained in two different experiments.
Concentrations observed at 25 mL/h: mean of the five last samples = 1204 mg/L (The relative difference = 18.29% : less than 30% as required by the OECD 105 - elution column method)
Concentrations observed at 12.5 mL/h: mean of the five last samples = 1132 mg/L (The relative difference = 7.79 % : less than 30% as required by the OECD 105 - elution column method)

Preliminary test

The approximate solubility determined by the preliminary test was between 1 and 10 g/L.

First experiment at a flow rate of 25 mL/h

The concentrations obtained as a function of time during this first experiment at 25 mL/h are presented in graph 1 : "Concentrations observed at 25 mL/h"

Measured pH :

-       at the beginning of the experiment : 5.5

-       at the end of the experiment : 7

The mean ± standard deviation of the five last samples is 1204 ± 82 mg/L.

 

The maximum difference observed in the five last samples is

           1337 - 1113 = 224 mg/L

 

The mean of these two maximum values is

           (1337 + 1113) / 2 = 1225 mg/L

 

The relative difference, corresponding to the ratio of the maximum difference and the mean of the two maximum values is

           224 / 1225 = 18.29%

The five last sample concentrations do not differ by more than + 30%, which means that equilibrium was established.

 

Second experiment at a flow rate of 12.5 mL/h

The concentrations obtained as a function of time during this second experiment are presented in graph 2 : "Concentrations observed at 12.5 mL/h".

Measured pH :

-       at the beginning of the experiment : 5

-       at the end of the experiment : 7

 

The mean ± standard deviation of the five last samples is 1132 ± 41 mg/L

 

The maximum difference observed in the five last samples is

           1174 – 1086 = 88 mg/L

 

The mean of these two maximum values is

           (1174 + 1086) / 2 = 1130 mg/L

 

The relative difference, corresponding to the ratio of the maximum difference and the mean of the two maximum values is

88 / 1130 = 7.79%

 

The five last sample concentrations do not differ by more than+30%, which means that equilibrium was established.

Conclusions:

The mean of the two solubility values obtained in the two different experiments is (1204 + 1132) / 2 = 1168 mg/L.
Interpretation of results: easily soluble (1 g/L - 10 g/L)
The relative difference between the results of the two experiments is (1204 – 1132) / 1168 = 6.16%.
The mean values obtained from two experiments did not differ by more than 30%, so these results are valid.

Executive summary:

The determination of the water solubility of dihydroterpineol multiconstituent was performed using the column elution method (OECD Guideline 105).

Due to the physicochemical properties of the test item (stability, volatility, adsorption on glass), the samples were analyzed as soon as possible after sampling. This precaution is crucial in order to avoid underestimation and variations of the measured concentrations.

Two independent experiments were carried out. The concentration of the substance was regularly measured by GC-FID (Gas Chromatography with flame ionization detector). The water solubility was recorded when the concentration reached a plateau.

The water solubility of dihydroterpineol multiconstituent obtained by the column elution method is 1168 mg/L. This value is the mean of two independent measurements.

Reference 2

Endpoint:

water solubility

Type of information:

experimental study

Adequacy of study:

key study

Study period:

13 June 2013 - 19 June 2013

Reliability:

2 (reliable with restrictions)

Rationale for reliability incl. deficiencies:

other: see "Remark"

Remarks:

The determination of water solubility was performed using the slow stirring method adapted from OECD Guideline No 123. This study was considered as reliable with restrictions because not enough details on quantification of the substance were reported in the report.

Reason / purpose for cross-reference:

reference to same study

Reason / purpose for cross-reference:

reference to other study

Qualifier:

according to guideline

Guideline:

other: adapted from OECD Guideline 123

Deviations:

no

Principles of method if other than guideline:

In a stirring vessel maintained at 20 +/- 0.5°C, ultra-pure water covered by a thin layer of the test item (~2 mm thickness) is slowly stirred. The speed was adjusted so that a minimal vortex is formed. The aim of this method is to prevent the formation of emulsions when saturating water. That can occur with the shake flask method and lead to a solubility overestimation. The water solubility is given by the mass concentration in water when a plateau as a function of time is reached. A second experiment is performed in the same conditions

GLP compliance:

no

Type of method:

other: slow-stirring method

Key result

Water solubility:

ca. 1 242 mg/L

Temp.:

20 °C

pH:

>= 7 - <= 8.55

Remarks on result:

other: Mean of two solubility values obtained in two different experiments.

Details on results:

First experiment : mean of the five last samples = 1248 mg/L (The relative difference = 5.96% : less than 15% as required by the OECD 105 - flask method)
Second experiment : mean of the five last samples = 1236 mg/L (The relative difference = 6.40% : less than 15% as required by the OECD 105 - flask method)

Preliminary test

The 10 mg sample was not fully dissolved in 10 mL of water.

The approximate solubility determined by the preliminary test was between 1 g/L and 10 g/L.

First experiment

The concentrations obtained as a function of time during this first experiment are presented in graph 1 : "Concentrations observed- first experiment"

Measured pH :

-       at the beginning of the experiment : 7

-       at the end of the experiment : 8.5

The mean ± standard deviation of the five last samples is 1248 ± 31 mg/L (The relative difference = 5.96% : less than 15% as required by the OECD 105 - flask method)

 

The maximum difference observed in the five last samples is

           1279 - 1205 = 74 mg/L

 

The mean of these two maximum values is

           (1279 + 1205) / 2 = 1242 mg/L

 

The relative difference, corresponding to the ratio of the maximum difference and the mean of the two maximum values is

           74 / 1242 = 5.96 %

 

Second experiment

The concentrations obtained as a function of time during this second experiment are presented in graph 2 : "Concentrations observed- second experiment".

Measured pH :

-       at the beginning of the experiment : 7

-       at the end of the experiment : 8.55

 

The mean ± standard deviation of the five last samples is 1236 ± 29 mg/L (The relative difference = 6.40 % : less than 15% as required by the OECD 105 - flask method)

 

The maximum difference observed in the five last samples is

           1274 – 1195 = 79 mg/L

 

The mean of these two maximum values is

           (1274 + 1195) / 2 = 1235 mg/L

 

The relative difference, corresponding to the ratio of the maximum difference and the mean of the two maximum values is

79 /1235 = 6.40 %

 

Conclusions:

The mean of the two solubility values obtained in the two different experiments is (1236 + 1248) / 2 = 1242 mg/L
Interpretation of results: easily soluble (1 g/L - 10 g/L)
The relative difference between the results of the two experiments is (1248 – 1236) / 1242 = 0.97 %

Executive summary:

The determination of the water solubility of dihydroterpineol multiconstituent was performed using the slow stirring method adapted from OECD 123 guideline.

Due to the physicochemical properties of the test item (stability, volatility, adsorption on glass), the samples were analyzed as soon as possible after sampling. This precaution is crucial in order to avoid underestimation and variations of the measured concentrations.

Two independent experiments were carried out. The concentration of the substance was regularly measured by GC /FID (Gas Chromatography with flame ionization detector). The water solubility was recorded when the concentration reached a plateau.

The water solubility of dihydroterpineol multiconstituent obtained by the slow-stirring method is 1242 mg/L.

This value is the mean of two independent measurements.

Description of key information

The water solubility of dihydroterpineol multiconstituent determined using the column elution method (OECD Guideline 105) is 1168 mg/L.

The water solubility of dihydroterpineol multiconstituent obtained by the slow-stirring method is 1242 mg/L.

The mean of these two results is 1205 mg/L.

Key value for chemical safety assessment

Water solubility:

1 205 mg/L

at the temperature of:

20 °C

Additional information

Key studies conducted according to OECD guideline 105 and an adaptation of OECD guideline 123. The results are scientifically acceptable but not obtained under GLP. Therefore a reliability of 2 (reliable with restrictions) was assigned.