Registration Dossier

Diss Factsheets

Physical & Chemical properties

Water solubility

Currently viewing:

Administrative data

Link to relevant study record(s)

Reference
Endpoint:
water solubility
Type of information:
experimental study
Adequacy of study:
key study
Study period:
Experimental Starting Date: 10 July 2014 Experimental Completion Date: 04 September 2014
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Remarks:
Study conducted in compliance with agreed protocols, with no or minor deviations from standard test guidelines and/or minor methodological deficiencies, which do not affect the quality of the relevant results. The study report was conclusive, done to a valid guideline and the study was conducted under GLP conditions.
Qualifier:
according to guideline
Guideline:
EU Method A.6 (Water Solubility)
Version / remarks:
slow stir adaptation of the standard method
Principles of method if other than guideline:
The water solubility of Shell GTL Solvent GS215 at 20.0 ± 0.5 °C was evaluated using a slow stir adaptation of the standard test method, based on the findings of Letinski, D.J., Connolly, M.J., Peterson, D.R. and Parkerton, T.F. (2002) “Slow-stir water solubility measurements of selected alcohols and diesters”, Chemosphere 48, 257-265. The method employed was designed to be compatible with the data endpoint requirements of Method A6 Water Solubility of Commission Regulation (EC) No 440/2008 of 30 May 2008 and Method 105 of the OECD Guidelines for Testing of Chemicals, 27 July 1995.
GLP compliance:
yes
Type of method:
other: slow stir adaptation of the standard method
Water solubility:
< 0 g/L
Temp.:
20 °C
Remarks on result:
other: Initial Nominal Loading Rate of 100 mg/L
Water solubility:
< 0 g/L
Temp.:
20 °C
Remarks on result:
other: Initial Nominal Loading Rate of 10 mg/L

Results

Main Test

The mean peak area ratios relating to the standard, sample and blank solutions are shown in the following tables:

 

Table 3.1– Nominal 100 mg/L Loading Rate

Solution

Mean Peak Area Ratio

Standard 10.8 mg/L

1.1473

Standard 10.1 mg/L

1.0771

Vessel 1 Sample 1

0.12275

Vessel 2 Sample 1

0.085385

Vessel 3 Sample 1

0.046270

Sample Blank

0.0032304

Standard 11.0 mg/L

1.1922

Standard 11.8 mg/L

1.3038

Vessel 1 Sample 2

0.067474

Vessel 1 Sample 3

0.046431

Vessel 2 Sample 2

0.061652

Vessel 2 Sample 3

0.027280

Vessel 3 Sample 2

0.030694

Vessel 3 Sample 3

0.048124

Sample Blank

0.0025111

Standard 11.3 mg/L

1.2304

Standard 12.1 mg/L[1]

1.1256

Vessel 1 Sample 4

0.00079501

Vessel 2 Sample 4

0.0065702

Vessel 3 Sample 4

0.0031705

Sample Blank

0.0095884

 

Table 3.1– Nominal 100 mg/L Loading Rate - Continued

Solution

Mean Peak Area Ratio

Standard 11.2 mg/L

1.1371

Standard 11.4 mg/L

1.2200

Vessel 1 Sample 5

0.047893

Vessel 1 Sample 6

0.00069220

Vessel 2 Sample 5

0.051351

Vessel 2 Sample 6

0.00081300

Vessel 3 Sample 5

0.059822

Vessel 3 Sample 6

0.0011707

Sample Blank

0.0019236

 

[1]Standard not used due to inconsistent response compared with other analyses.

Table 3.2– Nominal 10 mg/L Loading Rate

Solution

Mean Peak Area Ratio

Standard 10.8 mg/L

1.1473

Standard 10.1 mg/L

1.0771

Vessel 1 Sample 1

0.0091066

Vessel 2 Sample 1

0.0050910

Vessel 3 Sample 1

0.0079817

Sample Blank

0.0032304

Standard 11.0 mg/L

1.2074

Standard 11.8 mg/L

1.3067

Vessel 1 Sample 2

0.0075881

Vessel 1 Sample 3

0.0055487

Vessel 2 Sample 2

0.0074122

Vessel 2 Sample 3

0.0041110

Vessel 3 Sample 2

0.0088293

Vessel 3 Sample 3

0.0020043

Sample Blank

0.0025111

 

 

 

Table 3.2– Nominal 10 mg/L Loading Rate - Continued

Solution

Mean Peak Area Ratio

Standard 11.3 mg/L

1.2304

Standard 12.1 mg/L[2]

1.1256

Vessel 1 Sample 4

0.056688

Vessel 2 Sample 4

0.059110

Vessel 3 Sample 4

0.043786

Sample Blank

0.0095884

Standard 11.2 mg/L

1.2237

Standard 11.4 mg/L

1.2197

Vessel 1 Sample 5

0.0032338

Vessel 1 Sample 6

0.040415

Vessel 2 Sample 5

0.0064997

Vessel 2 Sample 6

0.029020

Vessel 3 Sample 5

0.0098106

Vessel 3 Sample 6

0.035627

Sample Blank

0.0019236

 

[1]Standard not used due to inconsistent response compared with other analyses.

As the test item peaks covered a wide retention time range and there were peaks observed in the blank solutions over the same range, the concentration attributed to the blank was subtracted from the sample concentrations. 

 

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

 

Table 3.3– Nominal 100 mg/L Loading Rate, Vessel 1

Sample Number

Stirring / Equilibration Time (hours)

Concentration (g/L)

Solution pH

1

42.3

1.11 x 10-5

6.66

2

114.0

5.87 x 10-6

6.68

3

119.8

3.97 x 10-6

6.90

4

137.0

-7.98 x 10-7

6.49

5

160.5

4.36 x 10-6

6.69

6

166.7

-1.17 x 10-7

6.82

 

A variable, negligible quantity was detected in the retention time range of the test item in both samples and sample blank. The amount detected was well below the range investigated for the analysis. The result is therefore taken as less than the level at which successful detection of the test item was achieved. See validation and discussion in overall remarks and attachments section below.

Table 3.4– Nominal 100 mg/L Loading Rate, Vessel 2

Sample Number

Stirring / Equilibration Time (hours)

Concentration (g/L)

Solution pH

1

42.3

7.65 x 10-6

6.81

2

114.0

5.35 x 10-6

6.70

3

119.8

2.24 x 10-6

6.89

4

137.0

-2.74 x 10-7

6.54

5

160.5

4.69 x 10-6

6.91

6

166.7

-1.05 x 10-7

6.45

 

A variable, negligible quantity was detected in the retention time range of the test item in both samples and sample blank. The amount detected was well below the range investigated for the analysis. The result is therefore taken as less than the level at which successful detection of the test item was achieved. See validation and discussion in overall remarks and attachments section below.

 

 

Table 3.5– Nominal 100 mg/L Loading Rate, Vessel 3

Sample Number

Stirring / Equilibration Time (hours)

Concentration (g/L)

Solution pH

1

42.3

4.01 x 10-6

6.71

2

114.0

2.55 x 10-6

6.61

3

119.8

4.12 x 10-6

6.70

4

137.0

-5.83 x 10-7

6.42

5

160.5

5.49 x 10-6

6.72

6

166.7

-7.14 x 10-8

6.51

 

A variable, negligible quantity was detected in the retention time range of the test item in both samples and sample blank. The amount detected was well below the range investigated for the analysis. The result is therefore taken as less than the level at which successful detection of the test item was achieved. See validation and discussion in overall remarks and attachments section below.

 

Table 3.6– Nominal 10 mg/L Loading Rate, Vessel 1

Sample Number

Stirring / Equilibration Time (hours)

Concentration (g/L)

Solution pH

1

42.3

5.47 x 10-7

6.92

2

114.0

4.54 x 10-7

6.84

3

119.8

2.71 x 10-7

6.81

4

137.0

4.28 x 10-6

6.41

5

160.5

1.13 x 10-7

6.72

6

166.7

3.51 x 10-6

6.41

 

A variable, negligible quantity was detected in the retention time range of the test item in both samples and sample blank. The amount detected was well below the range investigated for the analysis. The result is therefore taken as less than the level at which successful detection of the test item was achieved. See validation and discussion in overall remarks and attachments section below.

 

 

Table 3.7– Nominal 10 mg/L Loading Rate, Vessel 2

Sample Number

Stirring / Equilibration Time (hours)

Concentration (g/L)

Solution pH

1

42.3

1.73 x 10-7

6.91

2

114.0

4.38 x 10-7

6.72

3

119.8

1.42 x 10-7

6.69

4

137.0

4.50 x 10-6

6.42

5

160.5

4.12 x 10-7

6.73

6

166.7

2.47 x 10-6

6.44

 

A variable, negligible quantity was detected in the retention time range of the test item in both samples and sample blank. The amount detected was well below the range investigated for the analysis. The result is therefore taken as less than the level at which successful detection of the test item was achieved. See validation and discussion in overall remarks and attachments section below.

 

Table 3.8– Nominal 10 mg/L Loading Rate, Vessel 3

Sample Number

Stirring / Equilibration Time (hours)

Concentration (g/L)

Solution pH

1

42.3

4.43 x 10-7

6.84

2

114.0

5.65 x 10-7

6.94

3

119.8

-4.71 x 10-8

6.82

4

137.0

3.10 x 10-6

6.50

5

160.5

7.15 x 10-7

6.77

6

166.7

3.08 x 10-6

6.60

 

A variable, negligible quantity was detected in the retention time range of the test item in both samples and sample blank. The amount detected was well below the range investigated for the analysis. The result is therefore taken as less than the level at which successful detection of the test item was achieved. See validation and discussion in overall remarks and attachments section below.

 

The overall water solubility results for the two different loading rates evaluated are summarized in the following tables:

 

Table 3.9– Nominal 100 mg/L Loading Rate

Vessel

1

2

3

Mean Water Solubility (g/L at 20.0 ± 0.5 ºC)

< 1.20 x 10-4

< 1.20 x 10-4

< 1.20 x 10-4

Standard Deviation

not applicable

not applicable

not applicable

Relative Standard Deviation

not applicable

not applicable

not applicable

 

Overall water solubility                             :         less than 1.20x 10-4g/L at 20.0 ± 0.5 ºC

 

Table 3.10– Nominal 10 mg/L Loading Rate

Vessel

1

2

3

Mean Water Solubility (g/L at 20.0 ± 0.5 ºC)

< 1.20 x 10-4

< 1.20 x 10-4

< 1.20 x 10-4

Standard Deviation

not applicable

not applicable

not applicable

Relative Standard Deviation

not applicable

not applicable

not applicable

 

Overall water solubility                             :         less than 1.20x 10-4g/L at 20.0 ± 0.5 ºC

 


Conclusions:
Interpretation of results: insoluble (< 0.1 mg/L)
Please see Conclusion within the Executive Summary Section below.
Executive summary:

The determination was carried out using a slow stiradaptation of the standard test method, based on thefindings of Letinski, D.J., Connolly, M.J., Peterson, D.R. and Parkerton, T.F. (2002) “Slow-stir water solubility measurements of selected alcohols and diesters”, Chemosphere 48, 257-265. The method employed was designedto be compatible with the data endpoint requirements of Method A6 Water Solubility of Commission Regulation (EC) No 440/2008 of 30 May 2008 and Method 105 of the OECD Guidelines for Testing of Chemicals, 27 July 1995.

 

The slow-stir procedure was used as during a previous study (Harlan Study Number 41304205) using the flask method, it was identified that excess, undissolved test item could not be successfully excluded from the saturated solutions. The slow stir method eliminated dispersion of the test item throughout the solution and thus allowed isolation of saturated solutions free from excess, undissolved test item suitable for analysis.

 

Slow-stirring therefore enables the solubilisation of the test item without the formation of potentially problematic micro-droplets. The alternative column elution method proposed by the guidelines for addressing substances of low solubility is poorly suited to liquid test items.

 

As the test item is a UVCB substance, the effect of initial loading rate was also evaluated during the definitive determination of water solubility, using initial nominal loading rates of 100 mg/L and 10 mg/L, in order to assess if this affected either the resulting aqueous concentration or the composition of the dissolved fraction.

   

Conclusion

The water solubility of the test item at 20.0 ± 0.5 °C was evaluated using a slow stiradaptation of the standard test method. The results are summarized in the following table:

 

Table 3.11

Initial Nominal Loading Rate

Water Solubility
 (g/L of solution at 20.0 ± 0.5 °C)

100 mg/L

< 1.20x 10-4

10 mg/L

< 1.20x 10-4

 

Description of key information

water solubility (whole substance): <0.1 mg/l at 20±0.5°C (measured). 
water solubility (individual constituents): <1E-04 - 1.5E-01 mg/l at 20°C (QSAR)

Key value for chemical safety assessment

Additional information

The substance is a hydrocarbon UVCB and the constituent hydrocarbons will exhibit a wide range of water solubility. Standard tests for this endpoint are intended for single substances and are not appropriate for this complex substance as the composition of the total dissolved hydrocarbons will be different from the composition of the parent substance. However, this endpoint can be characterised using quantitative structure property relationships for representative hydrocarbon structures that comprise the hydrocarbon blocks used to assess the environmental risk of this substance with the PETRORISK model (see Product Library in PETRORISK spreadsheet attached in Section 13).

The "whole substance" water solubility of Hydrocarbons, C12-C15, n-alkanes, isoalkanes, <2% aromatics was evaluated using a slow-stir method. The method was designed to be compatible with EU Method A.6 and OECD 105. Since the submission substance is a UVCB, the effect of initial loading rate was also evaluated during the definitive study using initial nominal loading rates of 100 mg/l and 10 mg/l to assess if resulting aqueous concentration or composition of the dissolved fraction were affected. The water solubility of Hydrocarbons, C12-C15, n-alkanes, isoalkanes, <2% aromatics was determined to be <0.1 mg/l at 20±0.5°C in both the 100 mg/l and 10 mg/l loading rates.

As a supporting information, the water solubility of each constituent has been predicted using a separately validated QSAR estimation method. The prediction method uses a fragment method and water solubility decreases with increasing carbon number. The prediction domain covers carbon chain length in the range C2-C15, it is therefore expected that water solubility for longer chain length (i.e. greater than C15) compounds will be lower than the predicted value for C15 atom. Thus the water solubility of the individual constituents is in the range <1E-04 mg/l - 1.5E-01 mg/l at 20°C.